bluuebunny/crossref_metadata_2025 huggingface dataset:
A 13C N.M.R. study of some disaccharides from algal polysaccharides
Authors: Miller IJ , Wong H , Newman RH
Published: September 2010

The acid hydrolysis of agar,
a partially methylated agar, and K-carrageenan initially gives the disaccharide resulting from
cleavage of the link between the anhydrogalactose and
the galactose units. A new method for isolating
these disaccharides on a preparative scale is described, and their 13C
n.m.r. spectra are listed and assigned.
The extraction of zinc(II) from chloride solutions by methyltrioctylammonium and methyltridecylammonium chlorides dissolved in chloroform and other diluents and a comparison with Aliquat 336
Authors: Daud H , Cattrall RW
Published: September 2010

Equilibrium constants for
the extraction of zinc(II) from 1.0 and 6.0 M HCl and from 6.0 M LiCl solutions
by methyltrioctylammonium and methyltridecylammonium chlorides in chloroform
are reported. Vapour phase osmometry studies show that methyltrioctylammonium
and methyltridecylammonium chlorides form weak dimers in chloroform and
isobutyl methyl ketone. The presence of water in the diluent decreases the
extent of dimerization. The aggregation in o-xylene
and cyclohexane is more extensive with larger aggregates being formed. The
extraction of zinc(II) from 1.0 M HCl by methyltridecylammonium chloride in
different diluents follows the order isobutyl methyl ketone > cyclohexane
> o-xylene > chloroform. At
higher reagent concentrations the effect of aggregation is observed in
reversing the order for cyclo- hexane and o-xylene.
Anomalous extraction behaviour is observed with isobutyl methyl ketone which
may be due to the extraction of a different species in this diluent.
Pyrrolizidine alkaloids - A carbon-13 N.M.R. study
Authors: Jones AJ , Culvenor CCJ , Smith LW
Published: September 2010

A carbon-13 n.m.r. data base on 30 pyrrolizidine
alkaloids (19 new) of the crotalane and senecane series and a group of alkaloids containing
non-cyclic ester functions is presented. Attention is focused on the effects of
macrocyclic ring size, some hydrogen bonding,
substituents and in particular of stereochemistry on the 13C n.m.r.
chemical shifts. Useful observations in the 13C-1H coupled
spectra of these molecules are described, which may be used as an aid in the
characterization of this group of alkaloids. Deuterium isotopic shifts have
been used in some highly oxygenated (hydroxyl) systems to confirm assignments.
A new structure for grantaline (6) is confirmed and
an alkaloid previously identified as crispatine (4)
is suggested to be a new diastereoisomer.
Chemistry of pyrrolic compounds. LI. Porphyrins with electron-withdrawing groups in the same pyrrolic ring: preparation of a pyridazinoporphyrin
Authors: Chaudhry IA , Clezy PS
Published: September 2010

The preparation and
properties of porphyrins bearing electron-withdrawing groups in the same
pyrrolic ring are described. The principal example studied is a
diformylporphyrin and this has been used to prepare a porphyrin containing a
fused pyridazine ring. The properties of this novel system are discussed.
Chemistry of the Coccoidea. X. Synthesis of the xantholaccaic acid B system and of related compounds
Authors: Cameron DW , Feutrill GI , Perlmutter P
Published: September 2010

Xantholaccaic
acid B dimethyl ester pentamethyl ether (6) and some related anthraquinones have been synthesized by regiospecific
Diels-Alder addition of the highly functionalized dienes (12) and
(27) successively
to 2,6-dichloro-1,4-benzoquinone. This
is the first synthesis of the ?-arylanthraquinone
skeleton characteristic of the water-soluble dyestuffs from lac insects.
A preparative and phosphorus-31 nuclear magnetic resonance study of the coordination of three phosphate based ligands to dioxouranium(VI)
Authors: Bakas AE , Hounslow AM , Lincoln SF , Maeji NJ
Published: September 2010

The three species [UO2{OP(OMe)(NMe2)2}4](ClO4)2,
[UO2{OP(OMe)2(NMe)}5] (C1O4)2 and [UO2{OPMe2Ph)]5]
(ClO4)2 have been isolated and their CD2Cl2
solutions studied by means of 31P n.m.r. An equilibrium between [UO2L52+
and [UO2L4]2+ exists in solutions of the first
two species. In solutions of the third species [UO2L5]2+
predominates and ligand exchange proceeds through a dissociative
D mechanism for which kex (285 K), characterizing
a single ligand, is 1830 � 250 s-1, ΔH‡ 82.15 � 1.8 kJ mol-1
and ΔS‡ 106 � 16 JK-1 mol-1.
Studies in heterocyclics: novel synthesis of 4,5-diarylimidazoles
Authors: Soni RP
Published: September 2010

A novel synthesis of substituted 4,5-diarylimidazoles from N-(arylmethylene) methylamine N-oxides
and cold aqueous ethanolic potassium cyanide is
reported. A mechanism for the reaction is suggested.
All the imidazoles have been screened for antibacterial, fungicidal
and insecticidal activity.
The alkaloids of Gastrolobium callistachys
Authors: Cannon JR , Williams JR
Published: September 2010

(S)-(+)-Nb-Methyltryptophan
[(+)-abrine](1),(S)-(+)-Nb-methyltryptophan
methyl ester(2),(S)-(+)-Nb,Nb-dimethyltryptophan
methyl ester (3) and methyl (S)-(+)-2-methyl-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole-3-carboxylate (6)
have been isolated from the leaves of Gastrolobium
callistachys Meissn. The structure of (6) has been confirmed by synthesis.
Solvent dependence, metal ion catalysis and base catalysis of nitrito to nitro linkage isomerization of pentaamminenitritocobalt(III)
Authors: Jackson WG , Lawrance GA , Lay PA , Sargeson AM
Published: September 2010

The spontaneous rate of nitrito to nitro isomerization of [(NH3),Co(ONO)]2+ spans two orders of
magnitude for 16 solvents studied. The volume of activation is small and negative (from - 3.5 to
-7 cm3 mol-1) for water, dimethyl sulfoxide, N-methylformamide and sulfolane. Combined with
the observation of negligible competitive solvolysis, and of an isokinetic plot of ΔH‡ against ΔS‡,
this indicates that isomerization is intramolecular in all solvents. The solvent dependence is interpreted
in terms of a dual-parameter equation involving terms for the Lewis basicities (DN) and
Lewis acidities and polarity (ET). By use of this approach both DN and ET of the solvents are shown
to be major contributing factors to reactivity. Further studies on base-catalysed nitrito to nitro
isomerizations reveal mild catalysis by F-, AcO- and Et3N in Me2SO. The metal ions HgZ+, Ag+
and Cd2+ also catalyse the isomerization in water [kHg 1.16 × dm3 mol-1 s-1, kAg 2.85 ×
dm3 mol-1 s-1, kCd 4.4 × 10-5 dm3 mol-1 s-1; ,μ 1.0 M (CIO4-), 25°C]. The lack of competition
by AcO-, NO3- and H2O in the Hg2+-catalysed isomerization reaction also implicates an intramolecular
process for this path. In acetone, the ions Hg2+, Ag+, Cd2+ and Zn2+ catalyse the
isomerization reaction with a rate law of the form
Kobs = Ks + Km[n+]
except for Ag+, where the rate law takes the form
Kobs = (ks + kK[Ag+])/(1 + K[Mn+])
with kAg = kK = 2.11 × dm3 mol-1 s-1, k = 1.74 × 10-4 s-1 and K = 12 ± 1 dm3 mol-1.
The limiting rate is ascribed to a high stability constant for the silver adduct intermediate. The
analogous RhIII and IrIII complexes also exhibit catalysis by Ag+ and Hg2+ in aqueous solution.
Organothallium compounds. XVIII. The effect of antimony pentafluoride and fluorosulfuric acid on the thallation of polyfluoroarenes
Authors: Deacon GB , Smith RNM
Published: September 2010

The polyfluoroarenes m-H2C6F4,
m-O2NC6F4H,
m- and p-BrC6F4H, (p-HC6F4)2, C6F5H,
1,3,5-F3C6H3 and m-FSO2C6F4H have been thallated by
thallic trifluoroacetate in fluorosulfuric acid in the presence of antimony
pentafluoride. Substantial dithallation of m-H2F4
and 1,3,5-F3C6H3 and slight trithallation of
the latter have been achieved. The products were identified by conversion into
the corresponding polyfluoroiodoarenes on reaction with aqueous sodium iodide.
From the reaction with pentafluorobenzene, pentafluorophenylthallium(III)
species have been characterized. 1,2,4,5-Tetrafluoro-3-methoxybenzene was
thallated by thallic trifluoroacetate in 1,2-dichloroethane in the presence of
boron trifluoride etherate, but C6F5H and p-MeC6F4H failed
to react.
Detection by mass spectrometry of hydrocarbon biradicals, pyridine and aniline in a flame ionization detector
Authors: Head M , McAllister T
Published: September 2010

The
mass spectra of ions of >
75 in an f.i.d.-type flame with
benzene additive have shown that hitherto undetected species of formulas CllH9+
and CI3H9+ are present, which may be
attributed to protonation of the biradicals
C11H8 and C13H8 by H3O+.
The remainder of the hydrocarbon ions present are attributable to protonation of aromatic compounds (e.g. naphthalene and
indene) which have been detected previously in premixed benzeneloxygen
flames by electron impact ionization.
Addition
of NH3 to the benzene sample suppresses all the hydrocarbon peaks of
m/z >
100 but generates new peaks of m/z 80 and 94, attributable to the protonation of pyridine and aniline. Aniline may be
generated by addition of NH2 radicals to benzene in the pyrolysis and reaction zones of the flame.
The chemistry of aryllead(IV) tricarboxylates. Reaction with enamines
Authors: May GL , Pinhey JT
Published: September 2010

The treatment of
1-morpholinocyclopentene (la) with p-methoxyphenyllead triacetate (2a) in chloroform provides a
simple high-yielding route to 2-(4-methoxyphenyl)cyclopentanone
(3a). This arylation reaction of enamines
has been investigated with a variety of substrates and a number of aryllead triacetates. The reaction has been found to be
very sensitive to steric effects and is thus a useful synthetic method in a
relatively small number of cases. Acetoxylation is a
major competing reaction with those enamines of
cyclic ketones which give a low to moderate yield of arylated
product.
The reduction of substituted 2,8-Dioxabicyclo[3,2,1]oct-3-ylmethyl methanesulfonates with lithium aluminium hydride
Authors: Dimitriadis E , Massy-Westropp RA
Published: September 2010

2,8-Dioxabicyclo[3,2,1]oct-3-ylmethyl methanesulfonates
undergo a two-step reduction with lithium aluminium hydride to yield
tetrahydrofuran derivatives. The reduction of the carbon-oxygen bond of the
acetal occurs with retention of configuration and the reaction then proceeds by
reduction of an intermediate epoxide. The success of the reaction depends on
the configuration of the methane-sulfonyloxy
group.
The infrared matrix isolation spectra of carbon dioxide. II. Argon matrices: the CO2 monomer bands
Authors: Irvine MJ , Mathieson JG , Pullin ADE
Published: September 2010

Evidence is presented that
the cause of the doubling of the infrared bands of CO2 in an argon
lattice is the presence of two types of acceptable sites for the CO2
molecule. The nature of these sites is discussed; it is concluded that the
sites are double substitutional sites, in which a CO2
molecule occupies the place of two adjacent argon atoms, and single
substitution sites, in which the CO2 molecule occupies the place of
a single argon atom. A CO2 molecule in a double substitutional
site is a more stable situation than a CO2 molecule in a single substitutional site: the former gives a higher v3
and lower v2 frequency than the latter.
Kinetic studies on the mechanism of the nitraminopyridine rearrangement
Authors: Deady LW , Korytsky OL
Published: September 2010

Rate data are reported for
the rearrangement, in 92% sulfuric acid at 30�, of a series of 4-X-2-nitra-minopyridines
(X = H, Me, Br, CI, MeO, CO2H) and of 4-methyl-2-nitramino(3-D)pyridine.
Values of pKa for second protonation of the corresponding pyridin-2-amines were also
measured and rate constants for nitration of the monoprotonated
pyridinamines were thereby calculated. The results
suggest that the rate-determining step occurs prior to formation of the
appropriate 3-and 5-nitro σ complexes. The nature of this step is not
clear, however, and a key role for the nitramine
itself is not proven by the current evidence.
The reduction of some o-nitrophenylazo dyes with glucose: a general synthesis of 2-Aryl-2H-benzotriazole 1-oxides
Authors: Rosevear J , Wilshire JFK
Published: September 2010

The
reduction of some representative o-nitrophenylazo dyes in ethanolic
alkali with glucose gives the corresponding 2-aryl-2H-benzotriazole 1-oxides in excellent yield. These 1-oxides are
rapidly reduced to the parent benzotriazoles at room
temperature by means of zinc dust/ethanolic alkali.
This
method provides a convenient preparation for 5-chlorobenzotriazoles, which are
otherwise readily dechlorinated by zinc dust under more vigorous conditions.
Synthesis of (±)-pluviatolide and (±)-isopluviatolide
Authors: Ganeshpure PA , Stevenson R
Published: September 2010

The structure 2-(4-hydroxy-3-methoxybenzyl)-3-(3,4-methylenedioxybenzyl)-γ-butyrolactonep,r oposed
for the dibenzylbutyrolactone lignan pluviatolide, is confirmed by an unequivocal synthesis.
The isomer, isopluviatolide (2), has also been synthesized.
The free-radical phenylation of isoquinolinium cation
Authors: Beveridge AJ , Dyall LK
Published: September 2010

Free-radical
phenylation of isoquinolinium
cation has been effected by photolysis of phenylthalliurn(III)di(trifluoroacetate)
in a trifluoroacetic acid solution of isoquinoline. Analysis (g.l.c. and h.p.l.c.) of the
isomeric phenylisoquinoline mixture showed that the
dominant product (81.1 %) was 1-phenylisoquinoline,
in accordance with two published theoretical predictions.
Applications of molybdenum-95 N.M.R. spectroscopy. VI. 95Mo and 13C N.M.R. of certain cis-dioxomolybdenum(VI) compounds and related species. The crystal and molecular structure of Bis(N,N-diethylhydroxylamido(l -)-O,N)- disulfidomolybdenum(VI) hemibenzene
Authors: Gheller SF , Hambley TW , Traill PR , Brownlee RTC , O'Conner MJ , Snow MR , Wedd AG
Published: September 2010

The 95MO n.m.r.
spectra of a series of compounds containing the fac-[MoVIO3] and cis-[ MoVIO2] units are reported, together
with those for the series [MoX2(R2NO)2] (X = O
or S; R = Et, PhCH2). Trends in the data are discussed. The
stereochemistry in solution of certain of the cis-dioxo species is assigned by means of 13C n.m.r.
spectroscopy. The crystal and molecular structure of [MoS2(Et2NO)2],0.5C6H6
has been determined by X-ray crystallography. The steric and electronic
requirements of the terminal sulfide ligands significantly affect the detailed
coordination geometry relative to that observed for the dioxo analogue [MoO2(Et2NO)2].
Crystal data: a 10.162(2), b 11.836(2), c 14.437(2) �, β 106.12(2)� P21/a; Z 4.
Synthesis of Bis(6-methylquinolin-8-yl)phenylarsine and tris(6-methylquinolin-8-yl)-arsine and certain of their bivalent palladium and zerovalent molybdenum complexes. Crystal and molecular structures of Dichloro- and Diiodo-[bis(6-methylquinolin-8-yl)phenylarsine]palladium(II)
Authors: Roberts GL , Skelton BW , White AH , Wild SB
Published: September 2010

The potentially tridentate
chelating agent bis(6-methylquinolin-8-yl)phenylarsine
(AsN2) and quadridentate
tris(6-methylquinolin-8-yl)arsine (AsN2) have been prepared from
6-methyl-8-lithio-quinoline and dichlorophenylarsine
or arsenic trichloride, respectively. Both ligands
behave as bidentates in complexes of the type [PdX2(AsN2)]
and [PdX2(AsN2)] (where X = Cl
or I) and as tridentates in [Mo(CO)3(AsN2)]
and [Mo(CO)3(AsN2)]. The crystal and molecular structures
of [PdCl2(AsN2)],CH2Cl2 and [PdI2(AsN2)]
have been determined by single-crystal X-ray analysis. The dichloro
complex crystallizes in space group P1 (Ci1; No.2) with a 9.963(3), b 8.555(3), c 16.102(7) �;
α 86.64(3), β 82.13(3), γ 85.84(3)�; U 1354.3(9) �3
and Z = 2. The structure was solved by heavy-atom methods and refined by least
squares to R 0.044 for 2530 'observed' reflections with 1>3σ(I). The coordination geometry of the
palladium(II) atom is pseudo-square-planar in which the potentially tridentate AsN2
is behaving as a bidentate only. There is no evidence of
interaction of the remaining 6-methylquinolin-8-yl group with the metal centre,
although a weak interaction between the solvent of crystallization and the
metal may be present. The diiodo complex similarly
crystallizes in the centrosymmetric triclinic space
group P1 (Cil ; No.2) with a 13.590(5), b 10.035(2), c 9.435(2) �;
α 102.68(2), β 90.10(2), γ 92.99(2)�; U 1253.5(6) �3
and Z = 2. Least- squares refinement led to a convergence with R 0.038 for 3461
'observed' reflections. The structure of this complex was similar to that of
the dichloro analogue.
On the molecular geometry of 1,2-Di(9-anthryl)ethanes. Crystal structures of two crystalline modifications of 1,2-Bis(10-acetoxy-9-anthryl)ethane
Authors: Becker H , Hall SR , Skelton BW , White AH
Published: September 2010

In order to define
molecular conformations, the crystal structures of two crystalline phases of
1,2- bis(10-acetoxy-9-anthryl)ethane have been determined by single-crystal
X-ray diffraction methods at 295 K. Both phases are monoclinic, P21/c.
For the 'α'-phase, a 7.609(2), b 14.469(3), c 11.358(3) � β, 96.39(2)�, Z 2. The final residual was 0.034
for 1341 'observed' reflections; the molecule is centrosymmetric about a
crystallographic inversion centre. For the 'β'-phase, a 31.264(15), b 5.248(3),
c 15.718(6) �,β
97.84(3)�, Z 4, the final residual was 0.052 for 972 'observed' reflections. In
this structure two independent, centrosymmetric molecules are found. In both
α- and β-form, the molecular conformation is thus 'stretched' rather
than 'eclipsed'. The packing patterns of the two modifications have been
correlated with their crystal luminescence properties.
N-(Carboxymethyl)-N-[2-(2,6-diisopropylphenyl)amino]-2-oxoethylglycine and analogues: Synthesis and characterization
Authors: Best MP , McKeown RH , Wong O
Published: September 2010

N-(Carboxymethyl)-N-[2-(2,6-diisopropylphenyl)amino]-2-oxoethylglycine
(DIS-IDA)* (2a) and two analogues have been successfully synthesized. The
synthesis involved a modified one-pot reaction with specific reaction
conditions to maximize yields. A general procedure for the isolation of the
products has been set out and the stability of compounds (2) is briefly
discussed. Characterization is reported with a view for use with 99mTc as radiopharmaceuticals.
Metal template reactions. XIV. Synthesis of macrocyclic metal complexes from 2,2'-(oxalyldiimino)bisbenzaldehyde and related oxamido aldehydes and ketones
Authors: Black DSC , Vanderzalm CHB , Wong LCH
Published: September 2010

Numerous macrocylic
nickel(II) complexes and occasional copper(II) and cobalt(II) complexes have
been obtained from template reactions of the dialdehydes (3a-c) with diamines
(4). Related complexes from the diketones (3d,e) were prepared in some cases
with difficulty, but pure complexes could not be obtained from reactions
incorporating the diketone (3h). The preparation and methylation of the diamine
(9) has been carried out but formylation of compound (11) could not be achieved.
Ruthenium carbonyl complexes. I. Synthesis of [Ru(CO)2(bidentate)2]2+ complexes
Authors: Black DSC , Deacon GB , Thomas NC
Published: September 2010

The complexes RU(CO)2Cl2L
[L = 1,l0-phenanthroline (phen) or 2,2'-bipyridyl
(bpy)] react with silver carboxylates to yield Ru(CO)2(OCOR)2L derivatives (R = Me
or CF3). Reactions of Ru(CO)2(OAc)2L and Ru(CO)2(OAc)2(phen) with
trifluoroacetic and trifluoromethanesulfonic acid
give Ru(CO)2(OCOCF3)2L
and Ru(CO)2(OSO2CF3)2(phen) respectively. In acetonitrile,
Ru(CO)2(OAC)2L complexes react
with trifluoromethanesulfonic acid to give [Ru(CO)2(MeCN)2L]
(O3SCF3)2. The complexes [RU(CO)2L2]2+,
[Ru(CO)2(phen)(bpy)]2+,
and [Ru(C02(phen)(tmp)]2+ (tmp =
3,4,7,8-tetramethyl-1,l0-phenanthroline) have been prepared by reaction of [Ru(CO)2- (MeCN)2L]2+
and/or Ru(CO)2(OSO2CF3)2
phen with an excess of the appropriate
bidentate ligand. A similar series of reactions has yielded Ru(C0)2(OAc)2(py)2,
[Ru(CO)2(MeCN)2(py)2] (O3SCF3)2,
and [RU(CO)2(py)2L]2+
from Ru(CO)2Cl2(py)2. Stereochemical
assignments have been made for all complexes.
Reduction potentials of thiuram disulfide/dithiocarbamate couples in acetone/water
Authors: Nichols PJ , Grant MW
Published: September 2010

Reduction potentials
relative to the saturated calomel electrode, E�, of a series of thiuram disulfide/ dithiocarbamate
couples have been measured in 30% v/v water in acetone and at ,μ 0.2 moll-1
(NaNO3) by a combination of potentiometric
measurements and equilibrium constant determinations for thiolate/disulfide
interchange reactions. E� values lie in the range -250 to -340 mV which place dithiocarbamates as intermediate between thiophenolate (E� - 540 mV) and ethylxanthate
(E� -206 mV) in reducing properties. The significant effect on EO of varying
the substituents on the nitrogen in the dithiocarbamates
correlates with the substituent effects on the acid dissociation constants of
the parent dithiocarbamic acid and with trends in the
half-wave potentials for metal-based oxidation and reduction of transition
metal dithiocarbamate complexes.
Micellar catalysis of organic reactions. IX. The reaction of sodium azide with activated aromatic halides and the subsequent decomposition of the initially formed aryl azide
Authors: Broxton TJ , Jakovljevic AC
Published: September 2010

The effect of micelles of
cetyltrimethylammonium bromide on the SNAr reaction of azide ions
with 1-halogeno-2,4-dinitrobenzenes and on the subsequent decomposition of the
aryl azide product has been measured. The nucleophilic aromatic substitution
reaction is shown to be subject to significant micellar catalysis whereas the
subsequent decomposition of the aryl azide is not.
The measurement of 1JCH values from broad-band decoupled 13C N.M.R. spectra: application to the spectral assignment of cis-Pinan-2-ol
Authors: Blunt JW , Steel PJ
Published: September 2010

1JCH
values, together with chemical shift data and definite information on the
number of protons attached to each carbon in a compound, are available from
just three spin-echo Fourier-transform 13C n.m.r. spectra by
employing the pulse sequence θ-τ-180�-τ-180�-f.i.d., in which the
broad-band proton decoupler is gated off during the first delay period, and
with τ
values of 6, 8 and 9 ms. The experimental time required for collecting
these three spectra will be somewhat less than the total
time
required for the usual procedures for obtaining the chemical shift data and for
attempting to obtain carbon multiplicity and 1JCH data. Recent
assignment problems with cis-pinan-2-ol
are unambiguously resolved by this technique.
Oxygen reduction on titanium-doped α-Fe2O3 electrodes in aqueous alkali
Authors: McAlpine NS , Fredlein RA
Published: September 2010

Cyclic voltammograms
for titanium-doped α-Fe2O3 electrodes in 0.1 M NaOH exhibited small reduction and re-oxidation peaks
negative of -0.4 V (s.h.e.) and for electrodes
initially held negative of this potential, the onset of the photocurrent
occurred at potentials well positive of Vfb.
These results are interpreted as due to the penetration of hydrogen into the
lattice. The activity for oxygen reduction increased with dopant
concentration and plots of steady-state log i against
V exhibited slopes of absolute value approximately 2RT/F negative of Vfb, >2RT/F for Vfb
< V < 0.3 V and < 2RT/F at more positive than 0.3 V. No oxygen
reduction current was observed for oxygen partial pressures less than c. 0.45 atm. This effect was independent of electrode potential, dopant concentration and almost independent of pH. The results are interpreted
in terms of the step
O2 + H20 + e- → HO2(ad)+ OH-
being rate-determining with
titanium donors mediating change transfer.
Cobalt(II), nickel(II) and zinc(II) complexes of 3,3'-[Ethane-1,2-diylbis(imino)]-bis(propanamide) in solution
Authors: Lim M
Published: September 2010

The interactions of
3,3'-[ethane-1,2-diylbis(imino)]bis(propanamide) (H2eip)
with cobalt(II), nickel(II) and zinc(II) ions in 0.1 mol 1-1 KNO3
at 25�C have been studied by means of potentiometry.
In addition, the nickel system has also been studied by means of spectrophotometry, infrared and 13C n.m.r.
spectroscopy. Equilibria (1) and (2) were found to
hold:
Ni2++H2eip↔Ni(H2eip)2+ (1)
Ni2++H2eip↔Ni(H2eip)2H+
For the other metal ions
only equilibrium (1) was observed experimentally. The values of the equilibrium
constants for cobalt, nickel and zinc are log K1 5.39, 7.59 and 5.05
respectively, and pK1'' 19.24 for
nickel. For Ni(H2eip)2+, three absorption maxima were
found at γmax 746, 595 and 367 nm
with εmax values 6.5, 6.9 and 11.5 cm-1
mol-1l. respectively; for Ni(eip), only
one absorption maximum at γmax 446 nm
with εmax 91.9 cm-1 mol-1
l. was observed.
Organolanthanoids. IV. Some reactions of Bis(polyfluorophenyl)ytterbium compounds
Authors: Deacon GB , Mackinnon PI , Tuong TD
Published: September 2010

From reactions of
bis(polyfluorophenyl)ytterbium compounds R2Yb (R = C6Fs
or p-HC6F4) with trans-Rh(CO)Cl(PPh3)2,
NiCl2(bpy) (bpy = 2,2'-bipyridyl), NiCl2(PPh3)2,
PtCl2(bpy)2 triphenyltin chloride, iodine and mercuric
chloride, the polyfluorophenyl derivatives trans-RRh(CO)(PPh3)2,
R2Ni(bpy), trans-(C6F5)2Ni(PPh3)2,
(C6F5)2,Pt(bpy), Ph3SnC6Fs,
C6F5I and (C6FS)2,Hg have been
obtained. Reduction to mercury metal accompanied formation of the last
compound. Carbonation of (C6F5)2Yb in
tetrahydrofuran followed by acidification yields pentafluorobenzoic acid and,
surprisingly, a significant amount of 2,3,4,5-tetrafluorobenzoic acid, in which
the aromatic hydrogen is substantially derived from tetrahydrofuran. Reaction
of (C6F5)2Yb with pentafluorobenzoic acid followed
by acidification also gives 2,3,4,5-tetrafluorobenzoic acid. Fluoride
elimination is less extensive and less specific in a similar reaction of YbI2.
The course of cyclic ethylene acetal formation from 7a-methyl-2,3,7,7a-tetrahydro-1 H-indene-l,5(6H)-dione
Authors: Brown RFC , Burge GL , Collins DJ
Published: September 2010

All attempts to convert the
dione (1a) [7a-methyl-2,3,7,7a-tetrahydro-1H-indene-1,5(6H)-dione] into the
5-monoacetal (8)
[5,5-ethylenedioxy-7a-methyl-4,5,6,7-tetrahydro-2H-inden-l(7aH)-one] by direct
ethylene acetal formation under mild conditions have led to complex mixtures
usually containing the required monoacetal (8),its
conjugated enone isomer (9), the diacetal
(5) and the 1-monoacetal (2). The diacetal (5)
readily forms a dimer (4) in the presence of anhydrous acid, but in dioxan containing aqueous sulfuric acid it is hydrolysed to the 5-monoacetal (S), isolated in 68% yield
after chromatographic separation from the dione (la). For preparative purposes
the most convenient and reliable method for the preparation of (8) is
conversion of (la) into the 1-cyanohydrin (34), formation of the corresponding
5-acetal (36), and elimination of HCN from the 1-cyanohydrin group with
pyridine; this gave the 5-monoacetal(8) in 66% overall yield.
Deuterium isotope effects in liquid-liquid phase diagrams: Water + phenol and water + 2-methylpropanoic acid systems
Authors: Fenby DV , Khurma JR , Kooner ZS , Smith RF
Published: September 2010

Phase-separation
temperatures Tp have been measured for the
systems H2O+C6H5OH, H2O+
C6H5OD, H20+ CsD5OD, D20+
C6H50H, D2O+ C6H5OD,
D2O+ C6DsOD, H2O+ (CH3)2CHCO2H
and D2O+ (CH3)2CHCO2H. For water+
2-methylpropanoic acid, the differences in the Tp-x
curves for the exchange and no-exchange systems are striking. For water + phenol,
on the other hand, the effect of deuterium-exchange reactions on the Tp-x curves is very small. The results for all
systems are in accord with the qualitative predictions of the Rabinovich theory, which accounts for deuterium isotope
effects in liquid-liquid phase diagrams in terms of hydrogen bond and London
dispersion interactions. Molar excess enthalpies and molar excess volumes at
300.15 K are reported for the system water + 2-methylpropanoic acid. The
results are compared with those for water + acetic acid.
Raman spectra of hydrated cadmium nitrate in the glassy and crystalline state
Authors: Carrick MT , James DW , Leong WH
Published: September 2010

Raman spectra for
polycrystalline samples of Cd(NO3)2.4H2O
and Cd(NO3)2.12H2O
are reported at room temperature and at 80 K. The spectra are compared with the
spectrum of the anhydrous salt. The nitrate ion has an almost regular bidentate
binding to the cadmium ion in Cd(NO3)2.4H2O,
and this is used, with the spectral data, to test the conclusions from normal
coordinate calculations.The Raman spectrum of Cd(NO3)2.4H2O. in the
glassy state is reported, and it is found that the main features of the
corresponding crystal are present in the glass. There are some additional features
more characteristic of solution spectra which can be associated with disorder
in the amorphous phase.
Structure in nitrate glasses: Raman spectra of TlNO3-Cd(NO3)2 glass and mixed crystal
Authors: Leong WH , James DW
Published: September 2010

The Raman spectra of the equimolar mixture of Cd(NO3)2
and TlNO3 in the glassy and crystalline states have been
measured over a range of temperatures. The alternative interpretations of the results
in terms of distinct anion sites or a continuum of cation distributions are
examined. Strong similarities between the spectra of the crystalline and glassy
states indicate that three anion sites predominate. In two of these, the
environment is dominated by either cadmium ions or thallium ions, whereas the
third appears to have a mixture of the two cations.
Synthesis of ketones and methanols containing pyridinyl and N-methylimidazolyl groups
Authors: Canty AJ , George EE , Lee CV
Published: September 2010

N-Methylimidazolyllithium
reacts with N-methylimidazole-2-carbaldehyde to form bis(N-methylimidazol-2-yl)methanol,
and with the esters ethyl N-methylimidazole-2-carboxylate and ethyl
pyridine-2-carboxylate to give bis(N-methylimidazol-2-yl)methanone,(mim)2CO, and (N-methyl-
imidazol-2-yl)(pyridin-2-yl)methanone, (Py)(mim)CO, respectively. The ketones react with N-methylimidazolyllithium to give
tris(N-methylimidazol-2-yl)methanol, (mim)3 COH,
and bis(N- methylimidazol-2-yl)(pyridin-2-yl)methanol (Py)(mim)2 COH, respectively.
Volume changes associated with zeolite ionic exchange
Authors: Bottomley GA , Evans JA
Published: September 2010

Aqueous suspensions of zeolite(4A) in the potassium and sodium forms have been
separately exchanged with Ca2+ at 25�C in a precision dilatometer to
measure the associated system volume change, ∆Vobs.
Similar experiments partially exchanged K+ into sodium zeolite(4A) and Na+ into potassium zeolite(4A). Tris(ethane-1,2-diamine)cobalt(III) chloride
was also exchanged with sodium zeolite(13X). For the
overall process ∆Vobs is small,
generally well under 10 cm3 per mole of incoming cation exchanged. The results are discussed
in terms of three contributions to the overall volume change: (i) the volume change of ionic replacement in the solution
external to the zeolite (this is available from the
known apparent molar volumes of the electrolytes); (ii) the small dimension
changes of the zeolite lattices on exchange; (iii)
the transfer of water between zeolite and the
solution phase.
Dissociation kinetics of metal complexes in acid. II. Copper complexes of linear polyamines
Authors: Weatherburn DC
Published: September 2010

The acid decomposition
kinetics of the monocopper complexes of 20 different
linear polyamines have been studied over a range of acid concentrations (0.025
to 0.5 mol dm-3), I 1.0 (NaNO3). Complexes which contain
only six-membered chelate rings reacted at a rate which is independent of acid
concentration. Complexes with five-membered chelate rings have rate constants
which show a non-linear dependence on H+ concentration. Activation
parameters have been determined for some complexes. A mechanism, in which the
breaking of the first copper-nitrogen bond or the subsequent protonation of the
nitrogen atom is the rate-determining step, is proposed.
Oxidative decarboxylation of some Bicyclo[4,1,0]hept-3-ene-1-carboxylic acids
Authors: Galloway N , Dent BR , Halton B
Published: September 2010

Treatment of the
bicyclo[4,1,0]hept-3-ene-1-carboxylic acids (8d-f) with lead tetraacetate
results in oxidative decarboxylation and formation of the 1-aryl-1-methylethyl
acetates (12a-c).
Diels-Alder additions of dimethyl acetylenedicarboxylate to sterically hindered cyclohexa-2,4-dienones. Formation and X-ray structure analysis of stereoisomeric bicyclo[2.2.2]octadienones
Authors: Becker H , Skelton BW , White AH
Published: September 2010

The Diels-Alder addition of
dimethyl acetylenedicarboxylate to sterically hindered 2,4-cyclohexadienones (spiro-quinol ethers) gives rise to stereoisomeric
bicyclo[2.2.2]octadienones. The structures of three
of these have been elucidated by single-crystal X-ray diffraction methods and
their 1H n.m.r. and electronic absorption spectral properties are
reported.
Halogenated terpenoids. XX. The seven monochlorocineoles
Authors: Carman RM , Fletcher MT
Published: September 2010

The seven
monochlorocineoles have been synthesized, separated and characterized. Initial
attempts to identify these compounds as pollutants in chlorinated water
supplies from eucalypt-vegetated areas are discussed.
Crystal structure of Bis(2,2':6',2''-terpyridyl)cobalt(II) perchlorate c. 1.3 hydrate
Authors: Figgis BN , Kucharski ES , White AH
Published: September 2010

The crystal structure of
the title compound, [CO(C15H11N3)2](ClO4)2.c.
1.3H2O has been determined by single crystal X-ray diffraction
methods at 295 K. The structure is described in terms of atetragonal
P42/n sub-lattice structure similar to that of [Co(terpy)2]I2.2H2O,
with a 8.86(1), c 20.19(2) �. Perchlorate orientation and
disorder, however, demand consideration of superlattice
structures in I 41/a//F41/d with 4 and 8 times the P41/n cell volume. The relationship between the general structural
features of the [Co(terpy)2] X2
salts is described and discussed. The cobalt-nitrogen(central, distal)
distances (2.03, 2.14 �) are the longest observed in the [Co(terpy)2]2+ system, and are consistent
with the unusually high magnetic moment of the salt (4.2 BM).
The preparation and spectroscopic properties of some di- and tri-substituted 1,3,5-triphenyl-2-pyrazolines and related 2-pyrazolines
Authors: Rivett DE , Rosevear J , Wilshire JFK
Published: September 2010

The effect of substituents
on the absorption and fluorescence properties of a number of di-and tri-para-substituted
1,3,5-triphenyl-2-pyrazolines, several substituted 1,3,5,5-tetraphenyl- and trans-l,3,4,5-tetraphenyl-2-pyrazolines,
and some 1,3-diphenyl-trans-3a,4,5,6,7,7a-hexahydro-4,7-
methano-1H-indazoles in cyclohexane and in methanol has been studied. Certain
electron-with-drawing substituents, namely, cyano, methylsulfonyl or methoxycarbonyl,
have a marked effect. Such substituents located (�) in the 1-phenyl ring give pyrazolines exhibiting blue fluorescence which is quenched
if a cyano group is also present in the 5-phenyl
ring, (B) in the 3-phenyl ring give fluorescent yellow compounds which can be
considered as dyes, and (c) in the 5-phenyl ring cause quenching of the
fluorescence (unless an electron-withdrawing group is also present in the
3-phenyl ring).
The chloroform/graphite and carbon tetrachloride/graphite interfaces : Monte Carlo calculations of their properties
Authors: Lane JE , Quint GL , Spurling TH
Published: September 2010

The Grand Canonical Monte
Carlo calculations of the properties of the chloroform/graphite and carbon
tetrachloride/graphite interface have been performed at temperatures of 231.2,
268.2 (chloroform only) and 323.2 K. Agreement with experimental results is good
for the chloroform/ graphite interface but less satisfactory for the carbon
tetrachloride/graphite interface.
Intramolecular catalysis of organic reactions. III. Hydrolysis of 5-Nitro-2-(trifluoroacetylamino)benzoic acid
Authors: Broxton TJ
Published: September 2010

The hydrolysis of
5-nitro-2-(trifluoroacetylamino)benzoic acid (2) has been studied over the pH
range 0-12. In acidic solution (pH 0-3.5), the hydrolysis occurs with
intramolecular general acid catalysis by the adjacent CO2H group. Between pH
3.5 and 8, a plateau is observed in the pH-rate profile, and this is
interpreted as acid catalysis by a water molecule of the breakdown of the tetrahedral
intermediate formed between (2) and another water molecule. In alkaline
solution (pH > 8), hydrolysis occurs with general acid-catalysed C-N bond
breaking. Catalysis by phosphate and borate buffers was observed in the pH
range 6-10. Phthalate buffers did not catalyse the
reaction. For phosphate and borate buffers, plots of buffer concentration
against rate showed a saturation phenomenon which was interpreted as indicating
a change from rate-limiting decomposition of the tetrahedral intermediate to
rate-limiting formation of the tetrahedral intermediate as the buffer
concentration was increased. The pKa of the acid group was found to
be about 2.5 as expected, but the pKa of the NH group is 10.4,
higher than expected. The reduced acidity of the NH group is attributed to
electrostatic effects of the adjacent ionized carboxy
group. Unlike for aspirin, intramolecular catalysis by the ionized carboxy group was not observed, a result, perhaps, of
intramolecular hydrogen bonding between the carboxylate ion and the adjacent NH
group. Such an interaction would be geometrically unfavourable for either
intramolecular general base or nucleophilic participation by the carboxylate
ion.
The exchange of pyridine on bis-pyridine adducts of square-planar nickel(II) complexes containing dithiocarbamate, xanthate, dithiophosphate and monothioacetylacetonate ligands. A nitrogen-14 magnetic resonance study
Authors: Sachinidis J , Grant MW
Published: September 2010

14N n.m.r. has been used to measure the rates of pyridine exchange of a series of bis pyridine adducts
of square-planar nickel(II) complexes containing dithiocarbamate, xanthate, dithiophosphate and
monothioacetylacetonate ligands. Substantial variations in the lability of the coordinated pyridine
are observed, k,, at 298 K varying from about 103 to 107 s-1. In the monothioacetylacetonate series
the lability of pyridine decreases as the electron withdrawing power of the substituents increases.
Both the lability and the sensitivity to substituent effects are greater than for the analogous acetylacetonate
derivatives. The relationship between the intrinsic Lewis acidity of the nickel(II) centre in
the parent square-planar complexes as measured by equilibrium constants for bis pyridine adduct
formation and the lability of pyridine in the adducts is explored.
Structural studies in the iron(III)/chloride/α,α'-diimine system. III. Crystal structures of Tris(2,2'-bipyridine)iron(II) μ-Oxo-bis[trichloroferrate(III)] and of 'Compound A', μ-Oxo-bis[cis-chlorobis(1 ,10-phenanthroline)iron(III)] chloride solvate
Authors: Healy PC , Skelton BW , White AH
Published: September 2010

The crystal structure of [Fe(bpy)3] [CI3FeOFeCI3] (1) has been determined by single-crystal X-ray
diffraction at 295 K, and refined by least squares to a residual of 0.058 for 2002 'observed' reflections.
Crystals are monoclinic, P21/c, a 9.616(3), b 26.264(6), c 13.821(7) Ǻ, β 99.68(2)°, Z4. In the cation,
Fe-N distances range from 1.956(9) to 1 .989(10) Ǻ; in the anion, Fe-Cl distances range from
2.196(5) to 2.225(5) Ǻ. Fe-O distances are 1.763(11) and 1.740(11) Ǻ, and the Fe-O-Fe angle is
148.9(7)°. Recrystallization of 'compound A' from methanolic aqueous solution yields crystals
with stoichiometry [{cis-Fe(phen)2Cl}2O]Cl2.nH2O( n ≈ 4.5) as established by structure determination
(hampered by serious disorder); R is 0.09 for 749 'observed' reflections. Crystals are orthorhombic,
Pcn2, a 18.05(1), b 13.83(1), c 10.481(6) Ǻ, Z 2. The Fe-N distances trans to each other
are 2.12(3) and 2.13(3) Ǻ; Fe-N distances trans to Cl and O are 2.20(2) and 2.28(2) Ǻ, respectively.
Fe-CI is 2.34(1) and Fe-O 1.787(6) A; Fe-O-Fe is 161(1)°. For crystals from aqueous solution,
an isomorphous but larger unit cell is obtained [2754(7), cf. 2616(3) Ǻ3]; it is believed that this is
a consequence of variable occupancy of the disordered solvent layers which lie parallel to bc between
the ionic species.
Organophosphorus compounds. XVIII. Synthesis of 2-Phenyl-2,3-dihydro-1H-1,2-benzazaphosphole 2-sulfide by pyrolysis of (2-Aminobenzyl)phenyldithiophosphinic acid
Authors: Collins DJ , Drygala PF , Swan JM
Published: September 2010

Reaction of 2-phthalimidobenzyl bromide (12b) with the dialkyl phenylphosphonites (13a-c) afforded
the corresponding alkyl phosphinates (14a-c) which upon hydrazinolysis yielded the respective
(2-aminobenzy1)phenylphosphinates (16a-c). Reduction of the phosphinates (16a) or (16b) with
lithium aluminium hydride gave (2-aminobenzyl)phenylphosphine (15), characterized by its conversion
into crystalline 2,3-diphenyl-1,2,3,4-tetrahydro-1,3-benzazaphosphori(n1e8 ). (2-Aminobenzyl)
phenylphosphine (15) was heated with sulfur in benzene under reflux for 30 min to give 80%
of (2-aminobenzyl)phenyldithiophosphinic acid (20) which when heated between 100-200° in vacuum
underwent elimination of hydrogen sulfide to yield 2-phenyl-2,3-dihydro-1H-l,2-benzazaphosphole
2-sulfide (22a). Several other new phosphorus compounds are described.
An attempt to prepare a 1H-1,2-benzazaphosphole derivative by photolysis of methyl benzylphosphonic
azide (7) was unsuccessful.
Applications of the intermolecular nuclear Overhauser effect. II. The operation of solute-site factors in the interaction of polar solutes with the solvent benzene
Authors: Smith GR , Ternai B
Published: September 2010

By considering the
technique involving the measurement of aromatic solvent-induced shifts, and the
models which have been proposed from the results of such measurements, it is
suggested that the use of the solvent-induced solute proton intermolecular
relaxation rate [(1/T1)solvinter]
is a better method to study local solvation of solute
molecules. Proton relaxation rates obtained for simple solutes in the solvent
benzene are analysed in terms of an interaction parameter I, which treats (1/T1)solvinter]
in terms of a proton-proton pair distribution function. The resultant
dependence between I and a calculated
measure of the local polarity of the observed solute is discussed in terms of
previously proposed models of solute-solvent interactions.
The preparation of C-methyl-substituted triazamacrocyclic ligands
Authors: Graham PG , Weatherburn DC
Published: September 2010

The C-methyl-substituted macrocyclic compounds 2-and 3-methyl-1,4,7-tritosyl-1,4,7-triazacyclodecane,
2-methyl-1,4,8-tritosyl-1,4,8-triazacycloundecane,
2,2-dimethyl-1,4,8-triazacycloundecane,
meso-2,3-dimethyl-1,4,8-tritosyl-1,4,8-triazacycloundecane and the compound
3,6,9-tritosyl-3,6,9- triazabicyclo[9.3.1]pentadecane have been prepared by the Richman and Atkins
method. The yields of the macrocycles are low, separation from co-products is
difficult, and detosylation requires more vigorous
conditions than for the non-methyl substituted compounds.
The fate of carbonyl-18O in the rearrangement of an acyloxycarbene to a 1,2-dione
Authors: Brown RFC , Browne NR , Eastwood FW
Published: September 2010

5-[carbonyl-18O]Benzoyloxy-2,2,5-trimethyl-1,3-dioxan-4,6-dione
(1) was prepared by benzoylation of 5-hydroxy-2,2-dimethyl-1,3-dioxan-4,6-dione
with [18O]benzoyl bromide followed by C-methylation.Flash vacuum pyrolysis of(1)
at 560�/0.01 mm gave 1-phenyl[1-180]propane-1,2-dione. The position of the
label was determined by infrared and mass spectrometry. Scrambling of oxygen to
the2-carbonyl group was
negligible.
The structures and energy minimization analyses of the macrotricyclic cage complex [Co(nosartacn)]3+ and its precursor [Co(taetacn)]3+
Authors: Taylor SG , Snow MR , Hambley TW
Published: September 2010

The crystal structures of (-)487-[Co(taetacn)] (ClO4)3 [taetacn = 1,4,7-tri(2-aminoethy1)-1,4,7-triazacyclononane]
and (+)490-[Co(nosartacn)] (S2O6)3/2.4H2O
(nosartacn = 9-nitro-1,4,7,11,14,19- hexaazatricyclo[7.7.4.24.14]docosane)
have been determined. Crystals of the former complex (1) are cubic, space group
P213, a 13.168(5) �,
whereas the latter (2) are orthorhombic, space group C2221, a 10.22(1), b 6.944(8), c 32.33(1) �.
The structures were refined by blocked-matrix least-squares methods to R
factors of 0.040 and 0.050 on 952 and 2318 F
respectively. The absolute configurations and conformations are described as Δ(λδ) for (1) and Λ(λδ) for (2). Molecular mechanics
studies of conformers of both complexes show that the solid-state geometries
are the most energetically favourable, and that other
possible conformers are destabilized by coupling of the five-membered chelate
rings through the tertiary nitrogen atoms.
Magnetic exchange in 2,2'-bipyridyliron(III) chloride
Authors: Figgis BN , Kucharski ES , Reynolds PA
Published: September 2010

The magnetic susceptibility
and anisotropy of cis-bis(2,2'-bipyridyl)dichloroiron(III)
tetrachloroferrate(III), cis-[Fe(bpy)2Cl2]+
[FeCl4]-, have been measured between 1.8 and 300 K at magnetic
fields up to 1 T. The magnetization on the cation and anion sites has been
estimated by means of polarized neutron diffraction measurements at 1.5 and 4.6
T, and at temperatures from 2.1 to 41 K. These magnetic results may be fitted
to a 'mean-field' model of magnetic exchange in which the total exchange
integral parameter, ΣijJij, is c. -1.1 K. The
magnetic results and structural details for the compound suggest that the
strongest exchange pathway connects chains of alternating cations and anions.
The inter-chain exchange is small. However, the substantial magnetic anisotropy
and the much stronger decrease with temperature of the FeCl4- ion
site moment, relative to that of the cation, both indicate a complex magnetic
exchange network and consequent magnetic behaviour. No sign of magnetic order
is observed to at least 2.9 K.
Metal template reactions. XIX. Macrocyclic metal complexes derived from 2,2'-iminobisbenzaldehyde and some primary diamines with additional nitrogen donor atoms
Authors: Black DSC , Rothnie NE
Published: September 2010

Macrocyclic nickel(II), copper(II) and cobalt(II) complexes (6), (7), (9), (11), (13), (17) and (19) have
been prepared from 2,2'-iminobisbenzaldehyde, the appropriate metal salt and the primary diamines
3,3'-iminobispropylamine (4), 2,2'iminobisethylamine (9, 2,2'-(iminodimethylene)bisaniline (8),
azobenzene-2,2'-diamine (10), 2,2'-iminobisaniline (12), 2-amino-N-(2'-aminophenyl)benzamide (16)
and 2-amino-N-(2'-aminobenzoyl)benzamide (18) respectively. The nickel(II) complex (15), zinc(11)
complex (21) and copper(II) complex (22) were also prepared by similar methods. 2,2'-(Benzene-
1,2-diyldiimino)bisbenzaldehyde (25) was prepared but did not undergo metal template reactions to
allow the formation of macrocyclic complexes.
Metal template reactions. XX. Macrocyclic metal complexes derived from 4,6-Dimethoxy-3-methylindole-2,7-dicarbaldehyde and some primary diamines with additional nitrogen donor atoms
Authors: Black DSC , Rothnie NE , Wong LCH
Published: September 2010

4,6-Dimethoxy-3-methylindole-2,7-dicarbaldehyde
(6) has been prepared by the formylation of 4,6-dimethoxy-3-methylindole (5)itself
prepared by the hydride reduction of the oxoindole (4). Macrocyclic nickel(II)
and copper(II) complexes (8), (10) and (12) have been prepared from the dialdehyde (6), the appropriate metal(II) acetate and the
primary diamines 2,2'-iminobisaniline (7),
2-amino-N-(2'-aminophenyl)benzamide (9) and
2-amino-N-(2'-aminobenzoyl)benzamide (11) respectively.