bluuebunny/crossref_metadata_2025 huggingface dataset:
ÉTUDE QUANTITATIVE DES RÉACTIONS D'OZONOLYSE: II. OZONATION DU trans-STILBÈNE
Authors: Fliszár S. , Gravel D. , Cavalieri E.
Published: May 2006

The ozonolysis of 1 mole of trans-stilbene (in CCl4) by a stream of O2–O3 leads to the formation of 0.677 mole of stilbene ozonide, 0.468 mole of benzaldehyde, and 0.089 mole of benzaldehyde diperoxide. This ratio, observed for 80–100% ozonizations, is independent of the olefin concentration, the ozone flow rate, and the temperature (in the range 25–45 °C). These observations are explained, if one assumes that the reaction between two zwitterions can follow two courses: (a) formation of a dimer peroxide (55%), and (b) elimination of oxygen with the formation of two molecules of benzaldehyde (45%).
PARTITION COEFFICIENTS OF SOME CONJUGATED HETEROENOID COMPOUNDS AND 1,4-NAPHTHOQUINONES
Authors: Currie D. J. , Lough C. E. , Silver R. F. , Holmes H. L.
Published: May 2006

The concept of additive constants to predict the partition coefficient of a compound has been developed and applied to 244 compounds. Some of the limitations of such a concept are discussed.
THE SPECIFICITY OF HYDROGEN BOND FORMATION BETWEEN DERIVATIVES OF NUCLEIC ACID BASES AND SOME ANALOGUES
Authors: Pitha J. , Jones R. Norman , Pithova P.
Published: May 2006

Hydrogen bonding between pairs of derivatives of the base constituents of nucleic acids and their analogues has been studied in chloroform solution by infrared spectrophotometry. The strongest interactions occur between derivatives of guanine and cytosine. The introduction of the additional ring nitrogen atom in the pharmacologically active 5-azacytosine and 6-azacytosine derivatives does not change the complexing behavior. The positions of the N—H stretching bands in the infared spectra indicate that these complexes have a structure similar to that of the complexes formed between the corresponding pairs of bases in the naturally occurring desoxyribonucleic acid chain.
SYNTHESIS OF 6′-SUBSTITUTED MALTOSES
Authors: Dutton G. G. S. , Slessor K. N.
Published: May 2006

Derivatives of maltose substituted at position 6′ have been prepared by the replacement of a 6′-O-p-toluenesulfonate ester by various reagents. Tritylation of 1,6-anhydro-β-maltose followed by acetylation and detritylation yielded 2,3,2′,3′,4′-penta-O-acetyl-1,6-anhydro-β-maltose, which gave the 6′-O-p-toluenesulfonate in good yield. Replacement of the sulfonate ester with iodide led to a derivative from which 6′-deoxy-maltose was prepared by reduction, acetolysis, and deacetylation. 6′-Deoxy-6′-mercapto-maltose was prepared by replacement of the sulfonate with thiolacetate followed by acetolysis and deacetylation. 6′-Amino-6′-deoxy-maltose was prepared in low yield by azide replacement of the sulfonate, deacetylation, reduction, and mild acid hydrolysis.Attempts to prepare 6-substituted derivatives from benzyl 4′,6'-O-benzylidene-β-maltoside were unsuccessful. The possible explanations for the unreactivity of position 6 are discussed.
THE DIELECTRIC CONSTANT OF ETHYL CHLORIDE ADSORBED ON POROUS SILICA GLASS TREATED TO REMOVE SILANOL GROUPS
Authors: Shigeishi R. , McIntosh R.
Published: May 2006

The real and imaginary parts of the complex dielectric constant of the composite system ethyl chloride adsorbed on porous glass have been determined over a range of temperature, namely −20 to −190 °C in the frequency range 1 000 to 4 000 Mc/s. The porous glass was treated to remove the majority of the silanol groups. The dielectric constants of the adsorbate are also reported. The major finding was that removal of the silanol groups eliminated the second linear section (of lower slope) of the usual plots. The behavior of the polar adsorbate is then shown to be quite similar to that of polar adsorbates on nonporous rutile. Loss curves as functions of frequency and temperature are given and discussed. There is insufficient evidence to discriminate between Debye-type loss and that of an oscillator or resonator.A method is given of obtaining the dielectric parameters from the standing wave data with greater accuracy than can be obtained from use of Von Hippel plots.
CHARGE TRANSFER IN THE RADIOLYSIS OF BINARY HYDROCARBON MIXTURES
Authors: Stone J. A. , Quirt A. R. , Miller O. A.
Published: May 2006

The radiolysis of dilute solutions of ethane-dε, propane-d8, and n-butane-d10 in liquid hydrocarbons at 195 °K results in the production of D2 and HD in amounts which are determined by the relative ionization potentials of solvent and solute. Solvents of higher ionization potential enhance the production of D2 and HD from deuterated solutes of lower ionization potential. When the ionization potentials are in the reverse order the yields are diminished. This solute–solvent interaction, which is ionic in nature, is a general phenomenon in the radiolysis of mixtures of saturated hydrocarbons in the liquid phase and is consistent with charge transfer between solvent and solute.
REACTIONS OF ACTIVE NITROGEN WITH ORGANIC SUBSTRATES. IV. ISOPRENE
Authors: Hanafusa Terukyo , Lichtin Norman N.
Published: May 2006

not available
STEREOCHEMICAL STUDIES: VII. HYDROGENATION OF SOME STEROIDAL KETONES OVER ADAMS' CATALYST
Authors: Edward J. T. , Ferland J.-M.
Published: May 2006

The influence of the acidity of the solvent on the proportions of axial and equatorial alcohols obtained by hydrogenation of some steroidal ketones was investigated.
1,8-DIACETYLNAPHTHALENE AND 3-METHYLPHENALENONE
Authors: Tavares D. F. , Borger J. P.
Published: May 2006

not available
PARACHORS AND OTHER PROPERTIES OF ORGANOTINS
Authors: Putnam Robert C.
Published: May 2006

The parachors of a group of organotins were measured and compared with calculated values using both atomic constants and bond constants to obtain corresponding values for tin. The variation was found to be lower for the first method. The parachors were found to be about 8 times the molar refractions and could be approximately predicted from calculated molar refractions.The refrachors of the organotins were calculated and a suitable series of additive constants devised to approximate the found values. Excellent correlation was obtained between the order of refrachors corrected for molecular weight and the order of dispersions as expressed by the Nu (ν) values. An initial indication of alternation in methylene group increments for both molar refraction and Nu values was found. For a constant dispersion ratio (Q value) the refractive indices for the F and C lines of hydrogen were calculated.
ORGANIC COMPOUNDS OF SAMARIUM: II. REACTIONS OF SAMARIUM ISOPROPOXIDE WITH ETHYL ACETOACETATE
Authors: Sankhla B. S. , Kapoor R. N.
Published: May 2006

The reactions of samarium isopropoxide with ethyl acetoacetate have been carried out in benzene medium in different stoichiometric ratios and the compounds of the type Sm(OPri)2 (Etacac), Sm(OPri)(Etacac)2, and Sm(Etacac)3 have been isolated in quantitative yields. However, the reaction of samarium isopropoxide with excess of the acetoacetic ester lead to the formation of Sm(Etacac)3.Etacac, which on heating under reduced pressure at 110 °C for [Formula: see text] loses its addition molecule of ester. The reactions are exothermic and the amount of heat liberated also increases with the increase in the concentration of the ester.The interchange reactions of the products Sm(OPri)2(Etacac) and Sm(OPri)(Etacac)2 with t-butyl alcohol have also been carried out; they are endothermic reactions. The compounds Sm(OBut)2(Etacac) and Sm(OBut)(Etacac)2 have been obtained in quantitative yields from the reaction mixture. All the products are stable up to 200 °C at 0.5 mm, but at higher temperature they decompose to deep-red solids. Molecular weight determinations show that they are dimeric in nature.
A STUDY OF HINDERED DIARYLMETHYL RADICALS: II. THE BENZHYDRYL MODEL
Authors: Adam F. C. , Falle H. R.
Published: May 2006

This paper presents a model in which internal rotations of diphenylmethyl radical types effectively average out differences between the ortho and the meta substituent pairs in each ring. The process involves a very low energy of activation even though π-electron bonds are broken. The model is supported by valence bond (VB) and Huckel molecular orbital (HMO) calculations, and comparison is made with experimentally determined quantities wherever this is possible. Certain cases in which transannular pseudosymmetry has not been found are also discussed in relation to the above model.
THE PHOTOLYTIC AND PHOTOSENSITIZED DECOMPOSITION OF CHLOROFORM
Authors: Unger I. , Semeluk G. P.
Published: May 2006

The photolysis of CHCl3, in the vapor phase, was carried out using the 1 849 Å line of Hg as the exciting radiation. The photosensitized reaction was also studied using benzene as a photosensitizer. In the latter case, the exciting wavelength was the 2 537 Å line of mercury, which CHCl3 does not absorb.The study was primarily concerned with establishing the initial steps of the direct photolysis and photosensitized reactions. Experimental observations rule out a molecular detachment of HCl in both the direct photolysis and photosensitized reactions at the wavelength used. The initial step of the photolysis appears to be a carbon–chlorine bond cleavage, but in the photosensitized reaction a carbon–hydrogen bond break is indicated as the primary step. It is concluded that in neither case does dissociation take place from the ground electronic state.
RELATION BETWEEN ELECTRONS AND HOLES, AND THE VECTOR-COUPLING COEFFICIENTS FOR pmfq AND dnfq CONFIGURATIONS
Authors: Malli Gulzari L.
Published: May 2006

The electrostatic energy of an atomic state arising from a configuration involving holes differs by ΔW from the energy expression of the same state arising from the configuration involving electrons where ΔW can be expressed in terms of Slater's integrals.General formulas for ΔW are given for the pmfq and dnfq configurations. In addition, the vector-coupling (VC) coefficients useful for atomic self-consistent field (SCF) calculations are presented for all the states arising from the pmfq and dnfq configurations.
CHEMICAL DEACTIVATION BY HYDROCARBONS IN THE PHOTOLYSIS OF HEXAFLUOROACETONE
Authors: Khanna S. N. , Kutschke K. O.
Published: May 2006

not available
CHÉLATES DU GERMANIUM (IV) AVEC LA TROPOLONE, LE MALTOL, LA LAWSONE ET LA TRICHLOROHYDROXY p-BENZOQUINONE: II. NATURE ET STABILITÉ DES CHÉLATES
Authors: Beauchamp A. , Benoit R. L.
Published: May 2006

The formation of chelates between germanium (IV) and a series of α-hydroxyketones (HL) has been examined spectrophotometrically. Tropolone and maltol have been shown to give the species Ge(OH)2L2 and GeL3+; the corresponding equilibrium constants β2 and β3 have been determined. The following solid compounds have been isolated: Ge(OH)2(tropolonate)2•2H2O, Ge(tropolonate)3ClO4, and Ge(maltolate)3ClO4. There was no evidence of complex formation with lawsone and trichlorohydroxy p-benzoquinone. Relations are discussed between the chelate stability, the state of germanium (IV) in solution, and the acid–base properties of the α-hydroxyketones.
AN IMPROVED METHOD OF HYDROGEN ISOTOPIC EXCHANGE WITH DEUTERIUM SULFATE, AND THE PREPARATION OF 9,10-ANTHRAQUINONE-d8
Authors: Lunelli Bruno , Pecile Cesare
Published: May 2006

An apparatus and improved conditions are described for using easily and efficiently sulfuric acid-d2 as a deuterating agent. The preparation of 9,10-anthraquinone-d8 with a high deuterium content is reported.
PREPARATION AND CHARACTERIZATION OF SOME BINARY AND TERNARY METAL COMPLEXES OF IMIDAZOLE AND AMINO ACIDS
Authors: Rao G. N. , Li N. C.
Published: May 2006

Five new ternary metal complexes containing imidazole and glycylglycine or amino acid have been prepared and characterized by proton magnetic resonance and infrared spectral studies. Seven new binary metal complexes have also been prepared and studied. The isolation of Cd(imidazole)6Cl2•H2O and Ni(imidazole)6-Cl2•4H2O provides evidence that the coordination number of these metal ions to imidazole in the solid state is six. The visible spectra of the Ni(II) complexes of amino acid and imidazole show that all these are octahedral in aqueous solution.
STUDIES OF THE DISSOCIATION OF OXIDE SURFACES AT THE LIQUID–SOLID INTERFACE
Authors: Ahmed Syed M.
Published: May 2006

The dissociation of surface hydroxyl groups of crystalline SiO2, ZrO2, and ThO2, in aqueous suspensions, has been studied as a function of pHs at different ionic strengths of KNO3. The surface groups of quartz dissociate as weak acids, while those of ZrO2 and ThO2 dissociate amphoterically. A reversible double layer is formed at the oxide–solution interface, and H+ and OH− function as the potential-determining ions. Quantitative data have been obtained on (a) surface charge densities, (b) zero point of charge, (c) differential capacities of the double layer on quartz and ZrO2, and (d) the effect of surface charge density and ionic strength on the interfacial tension. The differential capacities indicate specific adsorption of NO3−on ZrO2 and ThO2 while NO3− has zero affinity for quartz surfaces. At low negative charge densities, solvated K+ are adsorbed on quartz and ZrO2 through coulombic interactions while at pHs > 10 specific adsorption of K+ predominates. ThO2 appears to exhibit a greater tendency for the specific adsorption of K+.
THE HYDROLYSIS OF DIMETHYLSULFATE AND DIETHYLSULFATE IN WATER
Authors: Robertson R. E. , Sugamori S. E.
Published: May 2006

not available
REARRANGEMENT OF ALLYL 2,6-DICHLOROPHENYL ETHER ON COLUMN PACKINGS DURING GAS–LIQUID CHROMATOGRAPHIC ANALYSIS
Authors: Baldwin M. J. , Brown R. K.
Published: May 2006

At temperatures above 175° and with packed columns, rearrangement of allyl 2,6-dichlorophenyl ether occurs during gas–liquid chromatographic analysis with a contact time of no more than 4 min. For example, at a temperature of 205° with Gas Chrom P as packing material, about 7% of the ether is changed, but the packing 20% Apiezon L on Gas Chrom P increases this to about 50%. Products characteristic of both thermal and acid-catalyzed rearrangements are obtained. The number of such products increases to a maximum of five as the temperature is increased to 228°.Accordingly, the results of gas–liquid chromatographic analysis of mixtures obtained from the Claisen rearrangement of allyl phenyl ethers must be interpreted with care if unchanged ether is present.
OXIDATION OF POLYSACCHARIDES BY LEAD TETRAACETATE IN DIMETHYL SULFOXIDE
Authors: Zitko V. , Bishop C. T.
Published: May 2006

Neutral polysaccharides can be oxidized by lead tetraacetate in dimethyl sulfoxide if 15–20% of glacial acetic acid is added to prevent oxidation of the solvent. The oxidation proceeds at a rate which is several times faster than that of periodate oxidation in aqueous solution, and the same amount of oxidant is consumed. Polysaccharides oxidized by lead tetraacetate in dimethyl sulfoxide can be recovered in excellent yield by precipitation with alcohol, and have been shown to contain free aldehyde groups. Identification of the products of reduction and hydrolysis of the oxidized polysaccharides showed that the oxidation followed the normal glycol-cleavage pattern given by lead tetraacetate in other solvents. Addition of potassium acetate to the oxidations in dimethyl sulfoxide decreased the consumption of lead tetraacetate by dextran (mainly α-(1 → 6) and α-(1 → 4)). Reduction and hydrolysis of dextrans oxidized in the presence and absence of potassium acetate yielded glycerol and erythritol in the respective ratios of 3.8:1 and 8.7:1. This result indicated that potassium acetate inhibited oxidation of the C-3, C-4 glycol groups in the dextran. Acidic polysaccharides behaved atypically in this oxidation system, and those containing a high proportion of uronic acid units were resistant to oxidation.
ÉTUDE DE LA FLUORESCENCE DES DÉRIVÉS DE LA PHÉNOTHIAZINE
Authors: Martin E. Adonai
Published: May 2006

not available
DERIVATIVES OF ISOTRITHIOCYANURIC ACID
Authors: Garmaise D. L.
Published: May 2006

A by-product isolated in low yield from the reaction of p-chlorobenzyl chloride with potassium thiocyanate and sodium iodide in dimethylformamide was shown to be the isotrithiocyanuric acid derivative I (R = p-chlorobenzyl). I gave the isodithiocyanuric acid ester (III) on alkaline hydrolysis, and mono-p-chlorobenzyl isotrithiocyanurate (IV) on reduction with sodium hydrosulfite. Treatment of I with sodium hypochlorite in aqueous alcoholic medium resulted in the direct replacement of the sulfhydryl group by an alkoxyl group. The N,S,S-triester VIII rearranged, on heating, to the symmetrical S,S,S-triester IX; this behavior is opposite to that shown by the oxygen analogues.
LIGNANS OF WESTERN RED CEDAR (THUJA PLICATA DONN): V. HYDROXYTHUJAPLICATIN METHYL ETHER
Authors: MacLean Harold , Murakami Koji
Published: May 2006

The structure of another guaiacyl–syringyl type lignan, which was previously separated from the hot-water extractive of western red cedar (Thujaplicata Donn), has now been determined as 2-hydroxy-2-(4″-hydroxy-3″,5″-dimethoxybenzyl)-3-(4′-hydroxy-3′-methoxybenzyl)-butyrolactone (III). This lignan is the third member of the thujaplicatin series and has been given the name of hydroxythujaplicatin methyl ether. Analytical data and degradational and spectral studies of the parent compound and its methylated derivatives are presented as proof of structure.
ÉTUDE CINÉTIQUE DE L'OXYDATION DE LA TRIBENZYLAMINE PAR LA N-BROMOSUCCINIMIDE
Authors: Zador Miklos
Published: May 2006

not available
ÉTUDES CONFORMATIONNELLES EN SÉRIE CYCLOPENTANIQUE: III. L'ADDITION DE DÉRIVÉS ORGANOMAGNÉSIENS SUR LA t-BUTYL-3 CYCLOPENTANONE
Authors: Richer Jean-Claude , Bélanger Patrice
Published: May 2006

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A NEW GALACTOBIOSYL GLUCOSE FORMED FROM LACTOSE BY CHAETOMIUM GLOBOSUM
Authors: Gorin P. A. J. , Haskins R. H. , Westlake D. W. S.
Published: May 2006

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ESTIMATED MOLECULAR WEIGHT OF AMYLOSE FROM THE YEAST RHODOTORULA PENEAUS
Authors: Gorin P. A. J. , Spencer J. F. T. , MacKenzie S. L.
Published: May 2006

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LA SYNTHÈSE DE QUELQUES NOUVELLES PYRIDAZINES BICYCLIQUES
Authors: Erichomovitch L. , Chubb Francis L.
Published: May 2006

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ORGANIC SULFUR COMPOUNDS III. CONDENSATIONS INVOLVING o-NITROBENZENESULFENYL CHLORIDE
Authors: Coutts R. T. , Hindmarsh K. W. , Pound N. J.
Published: May 2006

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MEAN MOLAL ACTIVITY COEFFICIENT RATIOS OF MIXED Na+–K+ SOLUTIONS OF p-TOLUENE AND POLYSTYRENE SULFONATES
Authors: Gamble Donald S. , Marinsky Jacob A. , Guptill Joel P.
Published: May 2006

A zeolite ion exchange technique for measuring mean molal activity coefficient ratios of mixed electrolytes has been further developed. The work was confined to systems of the type[Formula: see text]The 4A Zeolite has been calibrated for this kind of system by fitting the function[Formula: see text]to a fifth degree polynomial, in the range 0.1 ≤ XNa ≤ 0.7.Selectivity coefficient measurements with calibrated zeolite have been used to calculate ratios of mean molal activity coefficients for mixed Na+–K+ salts of model compounds. The model compounds were: p-toluene sulfonate, polystyrene sulfonate (mean molecular weight 400 000), and polystyrene sulfonate (mean molecular weight 30 000 to 40 000). The agreement between these measurements of activity coefficient ratios, and those calculated by Myers and Boyd for Dowex resins, ranges from excellent to fair.
FREE RADICALS BY MASS SPECTROMETRY: XXXIV. A FLOW REACTOR FOR MEASUREMENT OF FAST THERMAL REACTIONS
Authors: Fisher I. P. , Homer J. B. , Roberts B. , Lossing F. P.
Published: May 2006

A new type of flow reactor for use with a mass spectrometer has been constructed, in which many of the disadvantages of flow systems for rate measurements have been overcome. Rate constants for unimolecular decompositions can be measured in the range 50 – 5 000 s−1, with helium carrier gas pressures of 10–50 mm and residence times of 10−3 to 10−1 s. Measurements of the rate of thermal decomposition of trioxane are in good agreement with the rates predicted from literature data obtained at much lower temperatures.
THE RADIATION-INDUCED ADDITION OF HBr TO OLEFINS IN THE LIQUID PHASE
Authors: Rumfeldt R. C. , Armstrong D. A.
Published: May 2006

not available
MULTICOMPONENT DIFFUSION IN THE 85Kr–SO2–Kr SYSTEM
Authors: Saran Anil , Singh Yashwant
Published: May 2006

not available
A STUDY OF THE SUBSTITUTION REACTIONS OF BENZO[b]THIOPHENE AND ITS DERIVATIVES
Authors: Zyl Gerrit Van , Bredeweg C. J. , Rynbrandt R. H. , Neckers D. C.
Published: May 2006

The nitration, halogenation, and animation reactions of benzo[b]thiophene and some of its derivatives are reported. Several new benzo[b]thiophenes have been prepared and directional influences of groups in the thiophene portion of the nucleus confirmed.
THE WATER-SOLUBLE POLYSACCHARIDES OF DERMATOPHYTES: V. GALACTOMANNANS II FROM TRICHOPHYTON GRANULOSUM, TRICHOPHYTON INTERDIGITALE, MICROSPORUM QUINCKEANUM, TRICHOPHYTON RUBRUM, AND TRICHOPHYTON SCHÖNLEINII
Authors: Bishop C. T. , Perry M. B. , Blank F.
Published: May 2006

Polysaccharides obtained from each of the organisms designated in the title have been resolved into three groups: galactomannans I, galactomannans II, and glucans. The five galactomannans II were homogeneous under conditions of electrophoresis, and had positive specific rotations. Methylation and hydrolysis of the five galactomannans II yielded varying amounts of the following: 2,3,5,6-tetra-O-methyl-D-galactose, 2,3,4,6-tetra-O-methyl-D-mannose, 2,3,4-tri-O-methyl-D-mannose, 3,4,6-tri-O-methyl-D-mannose, 3,5-di-O-methyl-D-mannose, and 3,4-di-O-methyl-D-mannose. The galactomannans II were therefore very similar to each other in their gross structural features. The unbranched portions of the polysaccharides were formed by 1 → 2 and 1 → 6 linked α-D-mannopyranose units, with the former predominating. Branch points were formed through substitutions at the C-2 and C-6 positions of D-mannofuranose and D-mannopyranose, and branches were terminated by D-galactofuranose and D-mannopyranose units. The presence of 1 → 2 linked α-D-mannopyranose units in the linear portions of the galactomannans II constitutes a major structural difference between this group of polysaccharides and the galactomannans I. The two groups of galactomannans differ serologically.
SUBSTITUTIONS ÉLECTROPHILES EN SÉRIE NAPHTALÈNIQUE: III. SUR LE DI-t-BUTYL-2,7 NAPHTALÈNE
Authors: Erichomovitch Lucien , Ménard Marcel , Chubb Francis L. , Pépin Yvon , Richer Jean-Claude
Published: May 2006

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THE THERMAL REVERSIBILITY OF THE MICHAEL REACTION: V. THE EFFECT OF THE STRUCTURE OF CERTAIN THIOL ADDUCTS ON CLEAVAGE
Authors: Allen C. F. H. , Humphlett W. J.
Published: May 2006

A large number of Michael adducts have been prepared from β-morpholinoethanethiol and α,β-unsaturated compounds bearing a variety of functional groups. The extent of cleavage of 23 of these under reversal conditions has been determined quantitatively. The relation between structure and amount of cleavage has been discussed. A few heterocyclic thiols were also employed, to extend the generality of the reactions. With the latter, the thiol-cleaved product was separated and identified, to show that the cleavage was normal.
REARRANGEMENT STUDIES WITH 14C: XXVIII. SOLVOLYSES OF 1-14C-1-PROPYL p-TOLUENESULFONATE
Authors: Lee C. C. , Kruger James E.
Published: May 2006

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SYNTHESIS AND CHROMATOGRAPHIC PROPERTIES OF N-ALKYL-L-ASPARAGINES
Authors: Walter Roderich , Schwartz Irving L. , Trauth Louis J. , Berman Mervyn C. , Schlesinger David H.
Published: May 2006

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SOME STUDIES OF SLOW ROTATIONS AROUND BONDS IN AMIDES
Authors: Siddall III T. H. , Garner R. H.
Published: May 2006

Studies were made of the relative rates of rotation around the benzene-to-carbonyl, carbonyl-to-nitrogen, and nitrogen-to-benzene bonds in some α-naphthamides, o-substituted benzamides, and related compounds. In general bulky substituents on the nitrogen atom tend to increase the rate of rotation around the carbonyl-to-nitrogen bond, but to decrease the rate around the benzene-to-carbonyl bond. Naphthanilides with o-substitution in the benzene ring have a rapid rate of rotation around the naphthalene-to-carbonyl bond compared with other naphthamides. Relative rates of rotation can be rationalized on the basis of combined steric and electronic effects.
SOLVENT SHIFTS IN CHARGE-TRANSFER SPECTRA. INFLUENCE OF DONOR STRENGTH
Authors: Rosenberg H. M. , Eimutis E. , Hale D.
Published: May 2006

The charge-transfer transition energies for a series of methylbenzene–tetracyanoethylene complexes in four solvents are reported. The charge-transfer transition energies are found to decrease with increasing solvent refractive index. The magnitude of the decrease appears to be a function of donor strength. It is inferred that the excited state dipole moment decreases with increasing donor strength for these complexes.
HIGH RESISTANCE ANODIC OXIDE FILMS ON ALUMINIUM
Authors: Harkness A. C. , Young L.
Published: May 2006

The thicknesses of oxide films formed in aqueous borate solutions were obtained by the spectrophotometric method after developing the interference colors by evaporating a very thin film of gold or bismuth onto the oxide. The refractive index of the stripped films was determined by the Becke immersion method as 1.57 to 1.58 at 5 900 Å wavelength. The dielectric constant was estimated as 9.8 ± 0.5. Experimental data on the steady state ionic current density, I, through the oxide as a function of the field strength, E, in the oxide could be represented by I = I0 exp −(W − qaE)/kT where I0 = 2.24 × 107 A cm−2, W = 1.3 ± 0.15 eV, q = 3e, a = 2.95 ± 0.15 Å.
TETRASUBSTITUTED-CYCLOPENTADIENONE AND-p-BENZOQUINONE COMPLEXES OF RHODIUM(I)
Authors: McVey S. , Maitlis P. M.
Published: May 2006

The preparation of tetraphenylcyclopentadienone rhodium chloride, tetraphenylcylopentadienone rhodium carbonyl chloride, duroquinone rhodium chloride, and 2,3,5,6-tetraethyl-p-benzoquinone rhodium chloride from rhodium dicarbonyl chloride dimer and the appropriate organic ligand are described. The properties of these complexes and some of their reactions are discussed.
THE ELUCIDATION OF THE STRUCTURES OF OCHOTENSINE AND OCHOTENSIMINE
Authors: McLean Stewart , Lin Mei-Sie , Manske Richard H. F.
Published: May 2006

A combination of physical and chemical techniques has led unequivocally to the demonstration that ochotensimine and ochotensine have structures I and II, respectively.
THE ESSENTIAL OIL OF ILLICIUM ANISATUM LINN.
Authors: Cook W. B. , Howard A. S.
Published: May 2006

The oil of the Japanese star anise tree, Illiciumanisatum Linn., was analyzed by gas–liquid chromatography. The major constituents were found to be cineole (18.1%), linalool (10.1%), methyleugenol (9.8%), α-terpenyl acetate (6.8%), safrole (6.6%), and a sesquiterpene hydrocarbon of unknown constitution (7.2%). The composition of this oil differs widely from that of the commercially used star anise oil obtained from Illiciumverum Hooker. The most striking difference between the two oils is found in the anethole content, which constitutes 88% of the commercial oil but only 1.2% of the oil here investigated.
DEUTERIUM ISOTOPE EFFECT ON THE RACEMIZATION OF A HIGHLY HINDERED BIPHENYL DERIVATIVE
Authors: Heitner C. , Leffek K. T.
Published: May 2006

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CONVERSION OF NEOABIETIC ACID INTO MANOOL
Authors: Wenkert Ernest , Mahajan J. R. , Nussim M. , Schenker F.
Published: May 2006

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SYNTHESIS OF 6-METHYLCHOLESTA-3.5-DIENE; SOLVOLYSIS OF 6-METHYLCHOLESTERYL IODIDE
Authors: Just George , Lee-Ruff Edward
Published: May 2006

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A CONVENIENT METHOD FOR THE PREPARATION OF OPTICALLY ACTIVE BENZYL-α-d ALCOHOL
Authors: Wolfe Saul , Rauk Arvi
Published: May 2006

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CHLOROMETHYL–PHOSPHORUS COMPOUNDS SYNTHESIS AND INFRARED SPECTRA
Authors: Frank Arlen W. , Gordon Irving
Published: May 2006

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PHASE TRANSITIONS OF ADSORBATES: 1. SPECIFIC HEAT AND DIMENSIONAL CHANGES OF THE POROUS GLASS – WATER SYSTEM
Authors: Litvan G. G.
Published: May 2006

The specific heat and dimensional changes of the porous 96% silica glass – water system were measured simultaneously between −35 °C and +2 °C with coverages of 1.6, 4.0, 5.3, and 7.7 molecular layers. The specific heat of the adsorbate below the transition range was found to be higher than that of ice. No phase change was detected with the lowest concentration. At the higher coverages, transition always occurred near −9.5° and was of the anomalous first order type. The values of the specific latent heat of fusion, calculated by assuming that two monolayers do not freeze, are 49.4, 54.4, and 55.5 calg−1, depending on the concentration. The correlation between the results of calorimetric and dimensional change measurements was considered satisfactory.
CATALYTIC HYDRODESULFURIZATION OF THIOPHENE: VI. COMPARISONS OVER MOLYBDENUM DISULFIDE, COBALT MOLYBDATE, AND CHROMIA CATALYSTS
Authors: Kolboe S. , Amberg C. H.
Published: May 2006

The hydrodesulfurization of thiophene over five molybdenum disulfide catalysts, an alumina-supported cobalt molybdate, and a chromia catalyst has been investigated. Comparisons on the basis of equal surface areas showed that desulfurization activity did not vary a great deal. It was established mainly by working at very low conversion levels that 1,3-butadiene was a product over all these catalysts, and that a mixture of butadiene, the three n-butenes, and n-butane constituted the actual primary reaction product. The reaction rate is strongly dependent on conversion, probably as the result of small quantities of product H2S, the rate decreasing by a factor of 100 in going from 0.01% to 5% conversion in a typical flow experiment. A strong enhancement of the rate over MoS2 was noted in the presence of oxygen.
COORDINATION COMPOUNDS OF OLEFINS WITH ANHYDROUS SILVER SALTS: III. KINETICS OF THE GAS–SOLID REACTION PRODUCING AgBF4•2C3H6
Authors: Jull C. A. , Kominar R. J. , Mainland N. K. , Quinn H. W.
Published: May 2006

A study has been made of the pressure and temperature dependence of the rate of combination of propylene with silver tetrafluoroborate to produce AgBF4•2C3H6. Dependent upon the prior history of the salt, the reaction may proceed via predominantly diffusion control, predominantly kinetic control, or a combination of the two mechanisms. With both mechanisms, the adsorption of the olefin on the salt surface appears to exert a rate-controlling influence.
THE CORRELATION OF ABSORPTION SPECTRA AND STRUCTURE OF COPPER(II AND I)-2,2′-BIQUINOLINE COMPLEXES IN ACETONE MEDIA
Authors: Faye G. H.
Published: May 2006

A study of the absorption spectra of copper(II and I)-2,2′-biquinoline complexes in acetonic media has revealed that in the presence of excess ligand the predominant structure for both oxidation states of copper is probably that of a trigonal bipyramid. A crystalline monobiquinoline complex containing pseudo-octahedrally coordinated copper(II) has been isolated from solutions containing chloride ion. Evidence has been obtained that suggests the existence of a tris-biquinoline–copper(I) complex in which one biquinoline acts as a monodentate ligand.
STUDIES OF THE DISSOCIATION OF OXIDE SURFACES AT THE LIQUID–SOLID INTERFACE
Authors: Ahmed Syed M.
Published: May 2006

not available
PREPARATION AND CHARACTERIZATION OF SOME BINARY AND TERNARY COMPLEXES OF BENZOYLTRIFLUOROACETONE AND PHOSPHORUS ESTERS
Authors: Rao G. N. , Li N. C.
Published: May 2006

not available
THE INITIATION OF PROPYLENE PYROLYSIS
Authors: Marshall R. M. , Purnell J. H. , Shurlock B. C.
Published: May 2006

not available
35Cl AND 23Cl MAGNETIC RESONANCE OF SIMPLE CHLORINE COMPOUNDS
Authors: Saito Yasukazu
Published: May 2006

not available
THE CHEMISTRY OF YLIDS: XV. MECHANISM OF THE REACTION OF IMINOPHOSPHORANES WITH CARBONYL COMPOUNDS
Authors: Johnson A. William , Wong Simon C. K.
Published: May 2006

The pKa values of two series of iminophosphoranes, N-(substituted phenyl)-iminotriphenylphosphoranes (VI) and N-phenyliminotri-(substituted phenyl)-phosphoranes (VII), have been correlated with σ0 and σ, respectively, giving ρ values of +3.5 and +9.3. A kinetic study of the reaction of VI and VII with benzaldehydes indicates that a betaine intermediate (V) is involved. The rate-limiting step of the reaction changes, the result of a delicate balance between the nucleophilicity of the nitrogen atom and the electrophilicity of the phosphorus atom. The involvement of dπ–pπ bonding is indicated.
THE PREPARATION OF 4,6-O-BENZYLIDENE-D-GLUCAL AND THE REACTION OF METHYLLITHIUM WITH METHYL 2,3-ANHYDRO-4,6-O-BENZYLIDENE-α-D-ALLOPYRANOSIDE
Authors: Sharma M. , Brown R. K.
Published: May 2006

4,6-O-Benzylidene-D-glucal has been prepared by the reaction of benzaldehyde with D-glucal. The reaction of commercial methyllithium with methyl 2,3-anhydro-4,6-O-benzylidene-α-D-allopyranoside produces the C2-methylated 1,2-unsaturated compound 4,6-O-benzylidene-1,2-didehydro-1,2-dideoxy-2-methyl-D-ribo-hexopyranose. Their structures have been proven by first-order analyses of their nuclear magnetic resonance spectra.
METABOLITES OF PATHOGENIC FUNGI: V. ISOLATION AND TENTATIVE STRUCTURES OF VIOXANTHIN AND VIOPURPURIN, TWO COLORED METABOLITES OF TRICHOPHYTON VIOLACEUM
Authors: Blank F. , Ng A. S. , Just G.
Published: May 2006

Two new pigments, vioxanthin and viopurpurin, were isolated from Trichophytonviolaceum, and tentative structures are proposed. Xanthomegnin was found to be the major component of the pigment mixture.
CYCLIZATIONS OF DIALDEHYDES WITH NITROMETHANE: XIII. SYNTHESIS OF TREHALOSE-TYPE DISACCHARIDES CONTAINING NITROGENOUS HEPTULOSES
Authors: Baer Hans H. , Ahammad Alauddin
Published: May 2006

The dialdehyde II that arises from a partial lead tetraacetate cleavage of sucrose has been cyclized with nitromethane to give a stereoisomeric mixture of nitro disaccharides IV via their sodium nitronates III. Upon catalytic hydrogenation a single amino disaccharide, α-D-gluco-pyranosyl 4-amino-4-deoxy-β-D-gluco-heptulopyranoside hydrochloride (V), was isolated. Various derivatives of the nitrogenous heptulose components of IV and V were prepared by methanolysis and hydrolysis. The configuration of V was established by a degradation of its its N-acetylated hydrolysis product, 4-acetamido-4-deoxy-α-D-gluco-heptulose (VII), which gave 2-amino-2-deoxy-D-arabinose hydrochloride, and by reduction of VII, which gave the two epimeric acetamido heptitols XIII and XIV.
DERIVATIVES OF 4-AMINO-1-NAPHTHOL
Authors: Abdelkader M. A. , Khalifa M. , Abou-Zeid Y. M.
Published: May 2006

not available
DIIMIDE REDUCTION OF 12-MEMBERED CYCLIC OLEFINS
Authors: Nozaki H. , Simokawa Y. , Mori T. , Noyori R.
Published: May 2006

not available
THE KINETICS OF SORPTION AND DESORPTION OF WATER VAPOR BY LEAD STYPHNATE
Authors: Flanagan Ted B.
Published: May 2006

The kinetics of dehydration and rehydration of lead styphnate monohydrate have been studied as a function of the number of cycles of dehydration and rehydration. The activation energy for dehydration of a repeatedly dehydrated sample is 14.6 kcal/mole compared with 21.7 kcal/mole for the virgin hydrate. Mechanisms for these sorption and desorption phenomena are discussed.
PHOTOOXIDATION OF PROPIONALDEHYDE AT LOW PARTIAL PRESSURES OF ALDEHYDE
Authors: Altshuller A. P. , Cohen I. R. , Purcell T. C.
Published: May 2006

Propionaldehyde at partial pressures of from 0.0006 to 0.04 mm was photooxidized at 3 100 Å in the presence of 150 mm of oxygen. The major products were ethyl hydroperoxide and carbon monoxide. Acetaldehyde was formed at intermediate concentrations and formaldehyde, ethanol, methanol, hydrogen peroxide, and ethane were minor products. No ozone, peroxy acids, or diacyl peroxides could be detected.The results can be explained on the basis of a free-radical mechanism. Certain radical disproportionation reactions which are often postulated are unimportant because of the low partial pressures of propionaldehyde. An alternative mechanism involving direct chemical reaction of an oxygen molecule with the triplet state of the propionaldehyde may be of some significance, but cannot account for all of the products obtained. The present results indicate the importance of alkyl hydroperoxides as products in photooxidations at low partial pressures of aldehyde in the presence of large excesses of oxygen.
CHEMICAL REACTIONS IN ELECTRICAL DISCHARGES: II. THE STRUCTURE OF THE POSITIVE COLUMN IN D-C. GLOW DISCHARGES THROUGH FAST-FLOWING GASES
Authors: Peeters Jozef L. , Rundle Howard W. , Deckers Jacques M.
Published: May 2006

After a brief summary of recent advances in the structure of the positive column of a d-c. glow discharge, general expressions are derived for rates of reaction and excitation produced by electron impact. These rate equations are expressed in terms of the easily measured electrical parameters of the discharge. Such expressions will be used in future studies of chemical reactions occurring in the positive column; a qualitative comparison to experiment is given, where possible.A general expression for the axial electric field in the positive column is obtained by equating the energy gained by the electrons in this field to that lost by collisions. The main assumption made is that axial electron concentration be constant along the column.In the second part of the paper, calculations are done which indicate that ion and electron concentration gradients exist in the positive column adjacent to the anode. It is pointed out that such a phenomenon will be pronounced only under special conditions of low transverse and high axial field, and will be enhanced with fast-flowing gases.A sample calculation is presented using the expression for the rate of electronic excitation of a species by electron impact, assuming a Maxwell–Boltzmann energy distribution for the electrons and constant elastic and inelastic collision cross sections.
A STUDY BY ELECTRON PARAMAGNETIC RESONANCE SPECTROSCOPY OF RADICALS FORMED FROM ACETAMIDE AND FORMAMIDE
Authors: Smith P. , Wood P. B.
Published: May 2006

not available
Kinetics of the addition of acids to olefins with and without boron fluoride catalysis
Authors: Latrèmouille G. A. , Eastham A. M.
Published: May 2006

Isobutene reacts readily with excess trifluoroacetic acid in ethylene dichloride solution at ordinary temperatures to give t-butyl trifluoroacetate. The rate of the reaction is given, within the range of the experiments, by the expression d[ester]/dt = k[acid]2[olefin], and the apparent activation energy is about 6 kcal/mole. The rate of addition is markedly dependent on the strength of the reacting acid and is drastically reduced in the presence of mildly basic materials, such as dioxane. The boron fluoride catalyzed addition of acetic acid to 2-butene can be considered to follow a similar rate law, i.e. d[ester]/dt = k[acid·BF3]2[olefin], but only if some assumptions are made about the position of the equilibrium

[Formula: see text]since only the 1:1 complex is reactive.
Some reactions of triphenylmethyl compounds with boron fluoride
Authors: Burchill P. J. , Brownstein S. , Eastham A. M.
Published: May 2006

Triphenylmethyl derivatives, Ph3CX, where X = F, Cl, OH, or OCH3, react with 2 or more moles of boron fluoride to form Ph3CB2F7. Reactions take place rapidly and completely at low temperatures, except in the case of X = OCH3, where cleavage of the ether requires about 1 h at −30 °C. When X = Cl the other product is [Formula: see text]; for OH and OCH3 the products are B(OH)3 and B(OCH3)3·2BF3. The [Formula: see text] ion appears to be more stable than the [Formula: see text] or [Formula: see text] ions.
Étude quantitative des réactions d'ozonolyse. III. Note sur l'ozonation du diphényl-1,4 butène-2
Authors: Fliszár S. , Chylińska J. B.
Published: May 2006

The ozonization of 1,4-diphenyl-2-butene in CCl4 between 0 and 40° yields (on the average) 41.2% of ozonide, while 44% of the zwitterion not giving the ozonide is reduced.
Reactions of ozonides. V. Selective reduction of ozonides of 10-undecenoic acid derivatives by boranes
Authors: Diaper D. G. M. , Strachan W. M. J.
Published: May 2006

Borane–amine and tetrahydrofuran–borane adducts reduce 10-undecenoic acid ozonide and derivatives to 1,10-decanediol. Insufficient reagent allows selective reduction at the ozonide function, giving 10-hydroxydecanoic acid and derivatives through aldehyde intermediates. The reagents are not as selective as sodium borohydride. Thermochemical study shows an initial reaction step involving one molecule each of substrate and borane.
Accurate surface tension and charge determinations from polarographic drop-times
Authors: Barradas R. G. , Kimmerle F. M.
Published: May 2006

The precise determination of drop-times for micropolarographic mercury electrodes in aqueous inorganic electrolytes with and without the addition of organic surface-active compounds is described. A dependable mathematical method for conversion of drop-times to accurate surface tension data and the use of IBM computer techniques for the calculation of double layer parameters are discussed. Experimental results for hydrochloric acid, potassium chloride, and furfurylamine systems are reported.
The rhodium/selenium system
Authors: Rummery T. E. , Heyding R. D.
Published: May 2006

The rhodium/selenium system has been examined by room temperature X-ray powder diffraction patterns and by differential thermal analysis. A tentative phase diagram has been obtained. Eleven phases were observed, five of which were previously known. The compounds β-RhSe1.29, α-RhSe1.32, and α-RhSe1.34 have lattices based on the B81 structure; RhSe2+x and RhSe2.67 have defect pyrite lattices. The compound α-RhSe1.95 is isomorphous with IrSe2. The structures of RhSe1±0.1, β-RhSe1.34, α- and β-RhSe1.50, and RhSe1.9 are not yet known.
Infrared and Raman spectra of the cerium(IV) ion – nitrate ion – water system
Authors: Miller J. T. , Irish D. E.
Published: May 2006

Infrared spectra of aqueous solutions containing Ce(IV) and nitrate ions have been obtained by the attenuated total reflectance (a.t.r.) technique. Vibration frequencies and intensities have been measured and compared with infrared transmittance spectra and Raman spectra of both solutions and solids. The number of bands and the variation of band intensity with concentration changes indicate the presence of nitrato–cerium complexes in the solution. The polarization of the 1 538 cm−1 Raman band is advanced as a criterion that the coordination between the nitrate ion and the cerium(IV) ion is bidentate. Possible assignments are considered although many of the vibrations are characteristic of the ligand and hence are not diagnostic of a particular species.
The crystal and molecular structure of thioformaldehyde trimer
Authors: Fleming J. E. , Lynton H.
Published: May 2006

Crystals of thioformaldehyde trimer, (CH2S)3 are orthorhombic, space group Pmn21 with a = 7.697 Å

[Formula: see text], b = 7.067 Å

[Formula: see text], c = 5.323 Å

[Formula: see text]. There are two molecules in the unit cell with sulfur and carbon atoms in positions (4b) and (2a). The atomic parameters for sulfur and carbon have been determined from a three-dimensional analysis using observed and calculated differential syntheses with isotropic temperature factors. No absorption corrections were applied to the intensity data and no attempt has been made to establish the hydrogen positions. The final discrepancy index is R = 0.093. The molecule has the chair configuration and shows no significant difference between the lengths of any S—C bonds. The mean S—C bond distance is 1.818 Å and the standard deviation of the mean is 0.003 Å. This value is in good agreement with the commonly accepted value of 1.817 ± 0.005 Å for the S—C paraffinic bond.
Mass-spectrometric investigation of reaction of oxygen atoms with methane
Authors: Wong Edgar L. , Potter Andrew E.
Published: May 2006

A mass-spectrometric stirred-reactor technique was used to study the reaction of atomic oxygen with methane with low concentrations of molecular oxygen. An overall rate constant for oxygen-atom disappearance due to added methane was obtained for the temperature range 375 to 576°K. This rate constant was 4 × 1014 exp (− 10 000/RT) cm3 mole−1 s−1 and was compared with a previous rate constant for this reaction that had been measured in the presence of a large excess of molecular oxygen. This comparison showed that the presence of an excess of molecular oxygen produced a considerable increase in oxygen-atom consumption at low temperatures, but only a small increase at high temperatures. From product analyses, the stoichiometry of the reaction could be approximately represented by

[Formula: see text]From the reaction stoichiometry and the rate constant for the oxygen-atom disappearance, the rate constant for methane disappearance was calculated to be 1 × 1014 exp (− 10 000/RT) cm3 mole−1 s−1. The presence of excess molecular oxygen has very little effect on this rate constant, contrary to the result found for the disappearance of atomic oxygen.
Fully fluorinated alkoxides. Part II. Ethoxides, propoxides, and butoxides
Authors: Redwood M. E. , Willis C. J.
Published: May 2006

Ionic, fully fluorinated, ethoxides, n-propoxides, isopropoxides, and n-butoxides of the heavier alkali metals may be made by the reaction of the appropriate acyl fluoride, or of hexafluoroacetone, with the metal fluoride. Factors affecting the stability and possible synthetic use of such compounds are discussed, together with n.m.r. (nuclear magnetic resonance) and infrared spectral data.
Infrared studies on rotational isomerism. I. Ethylene glycol
Authors: Buckley Paul , Giguère Paul A.
Published: May 2006

The problem of the equilibrium configuration of the ethylene glycol molecule was investigated by measuring the infrared spectra of the vapor (up to 125 °C), liquid, and solid phases between 100 and 3 700 cm−1. The two isotopic molecules (CD2OH)2and (CH2OD)2were likewise studied. Most of the fundamental frequencies could be observed and assigned. These assignments, as well as the phase and temperature behavior of the spectra, confirm that in all cases the molecules exist only as gauche isomers, which are more stable than the trans as a result of intramolecular hydrogen bonds. Because these bonds are far from linear, the OH stretching vibrations are little affected, but the bending vibrations are strongly shifted towards higher frequencies.Comparison of the calculated thermodynamic functions with the calorimetric data shows that restriction of all three internal rotations in the glycol molecule lowers the entropy by about 10 e.u. at normal temperature. From the observed torsional frequencies, the average barrier heights are estimated to be of the order of 10 kcal/mole for rotation about the C—C bond, and 3 to 4 kcal/mole for rotation about the C—O bonds, thereby indicating a fairly rigid structure.
The synthesis of lα-methylcortisone and lα-methylhydrocortisone
Authors: Tanabe Masato , Crowe David F.
Published: May 2006

The addition of methylmagnesium iodide to 17α,20;20,21-bismethylenedioxy-1,5-pregnadiene-3,11-dione and 17α,20;20,21-bismethylenedioxy-1,4-pregnadiene-3,11-dione yields 1α-methyl derivatives. These derivatives can be converted further into 1α-methylcortisone and 1α-methylhydrocortisone. The isolation of a 3-methylene-Δ1,4 derivate is also described.
Structural biochemistry. IV. 3β-Hydroxy-17β-(l-prolyl)amino-androst-5-ene
Authors: Pettit G. R. , Smith R. L. , Gupta A. K. Das , Occolowitz J. L.
Published: May 2006

The synthesis of the title compound III was studied in detail and the following combination of methods was found reliable and convenient. The oxime derivative Ib of ketone la was reduced with sodium–ethanol to 3β-hydroxy-17β-amino-androst-5-ene. The configurational assignment for amine IIa was supported by the results of a comparison with the 17α-epimer and by a proton magnetic resonance study of both isomers. Selective reaction between amine IIa and carbobenzoxy-l-proline was achieved with Woodward's reagent K. Of several procedures explored for removing the carbobenzoxy protecting group from amide IIc, palladium-catalyzed hydrogenolysis proved quite satisfactory. Hydrogenolysis of carbamate IIb to yield prolyl amide III was realized without affecting the Δ5 olefin system. A mass spectral study of amine III and the corresponding 5α-derivative IV confirmed the latter observation. A brief review of procedures for the synthesis of steroidal amines was also presented.