bluuebunny/crossref_metadata_2025 huggingface dataset:
Folic acid analogs. III.N‐(2‐[2‐(2,4‐diarnino‐6‐quinazolinyl)ethyl]benzoyl)‐l‐glutamic acid
Authors: Yan S. J. , Weinstock Louis T. , Cheng C. C.
Published: April 2009

A trideaza analog of aminopterin,N‐(4[2‐(2,4‐diamino‐6‐quinazolinyl)ethyl]benzoyl)‐L‐glutamic acid, was prepared by a Wittig condensation of 2,4‐diaminoquinazoline‐6‐carboxaldehyde and [P‐(N‐[1,3‐bis(ethoxycarbonyl)propan‐1‐yl]aminocarbonyl)phenylmethyl]triphenylphosphonium bromide followed by catalytic reduction and mild hydrolysis. This compound was found to have confirmed inhibitory activity against leukemia L1210 in mice.
Totally synthetic steroid heterocycles. Part 7.. A facile approach to 16‐oxa‐D‐homoestrogens
Authors: Terasawa Tadao , Okada Toshihiko
Published: April 2009

In search of biologically active modified steroids, novel 16‐oxa‐D‐homoestrone and ‐D‐homoestradiol 3‐methyl ethers were synthesized from 16‐oxa‐3‐methoxy‐D‐homoestra‐1,3,5(10),8,14‐pentaen‐17a‐one. The straightforward synthesis involved stereoselective two‐step reduction of the 8,14‐diene system. The B/C stereoisomers were also derived from the estrapentaene. The stereostructures of these heterocyclic estrogens were determined on the basis of their spectral data.
The synthesis of heterocyclic derivatives of dibenzo[a,d]cycloheptene
Authors: Hollins Richard A. , Martins Paulo R. C.
Published: April 2009

The synthesis of 2‐amino‐7,8‐dihydrobenzo[1,2]cyclohepta[3,4,5‐de]quinazoline (10) and 6,7‐dihydrobenzo[1,2]cyclohepta[3,4,5‐cd]indazole (5) is described.
Synthesis and thermolysis of N‐heteroarylacetylazides and α‐oximino‐α‐(N‐heteroaryl)acetylazides
Authors: Iwao Masatomo , Kuraishi Tsukasa
Published: April 2009

Treatment of N‐heteroarylacethydrazides with an equimolar amount of nitrous acid afforded N‐heteroaryacetylazides and subsequent thermolysis of these azides gave the analogues of 2,3‐dihydroimidazo[1,5‐a]pyridin‐3‐one. When some of these cyclized compounds were treated with nitrous acid, the ring opening reaction occurred and recyclized 3‐(N‐heteroaryl)‐1,2,4‐oxadiazolin‐5‐ones were obtained. Treatment of N‐heteroarylacethydrazides with two equivalent moles of nitrous acid afforded α‐oximino‐α‐(N‐heteroaryl)acetylazides. Thermolysis of these azides gave mixtures of 3‐(N‐heteroaryl)‐1,2,4‐oxadiazolin‐5‐one and 3‐hydroxy‐4‐(N‐heteroaryl)furazan. On the basis of the effects of heterocyclic rings and solvents upon the relative yield of two types of the products, one plausible mechanistic explanation for the decomposition of such azides was proposed. α‐Oximino‐α‐(H‐heteroaryl)acetylazides were converted into cyano N‐heterocycles by the action of alkali in good yields.
Synthèse de dérivés de la benzo[c] quinolizine
Authors: Vierfond Jean‐Michel , Mettey Yvette , Joubin Raymond , Miocque Marcel
Published: April 2009

Pour introduire des centres polaires dans des systèmes pluricycliques plans en vue d'étudier leur action intercalante, on a préparé des dérivés de benzo[c]quinolizinium fonctionnalisés par un groupement OH ou NH2: les précurseurs cétoniques ou iminés sont obtenus à partir du picolyl‐2 ou du quinaldyllithium; ils subissent ensuite une cyclisation par quaternisation mettant vraisemblablement en jeu un processus concerté. La structure des composés obtenus et de certains de leurs dérivés est étudiée.
Fused indoles. 2. Synthesis and reactions of imidazo[1,2‐a]‐ and pyrimido[1,2‐a]‐indoles
Authors: Coppola Gary M. , Hardtmann Goetz E.
Published: April 2009

The alkylation of 2‐chloroindole‐3‐carboxaldehyde (1) and 3‐acetyl‐2‐chloroindole (5) with 3‐chloro‐N,N‐dimethyl‐1‐propylamine, 3‐chloro‐N,N‐diethyl‐1‐propylamine and 2‐chloro‐N,N‐dimethyl‐1‐ethylamine is described. Following alkylation, demethylation occurs and furnishes imidazo[1,2,‐a]‐ and pyrimido[1,2‐a]indoles (3a,6,8,10). Pyrimido‐indole 3a, on treatment with lithium aluminum hydride, furnishes the bis‐indole 12. Analogous reaction with diborane affords the reduced product 14, while reaction with methyllithium yields the deformylated product 13. Spectral data of the resulting compounds are also discussed.
Recherches en série diazépine‐1,4 et triazépine‐1,2,4. XV. Syntlièse d'halogéno‐3(7)‐s‐triazolo[4,3‐b] triazépinones
Authors: Essassi E. M. , Lavergne J.‐P. , Viallefont Ph.
Published: April 2009

L'halugénution de s‐triazolo[4,3‐b] triazépinones selon différentes méthodes a été réalisée. Selon les conditions expérimentales et les agents d'halogénation il a été possible d'halogéner le cycle triazépine (position 7) ou (et) le cycle triazole (position 3). Au total 18 halogéno s‐triazolo triazépinones ont ainsi été préparées et les structures établies a partir de l'ensemble des données spectrales.
Total synthesis of a B‐ring “homoalkaloid”. 4,5,6,7,7a,8‐Hexahydro‐7‐methylphenanthro[10,1‐bc]azepine
Authors: Jensen Bruce L. , Woods Michael A.
Published: April 2009

The synthesis of a novel benzazepine, 4,5,6,7,7a,8‐hexahydro‐7‐methylphenanthro[10,1‐bc]‐azepine, is described. Two pathways leading from 1,2,4,5‐tetrahydro‐1‐(o‐nitrophenyl)‐3H‐2‐benzazepin‐3‐one were investigated. The most successful route, utilizing a Pschorr cyclization followed by diborane reduction and Eschweiler‐Clarke methylation, led to an excellent yield of the title compound.
Substituted 2,3,4,5‐tetrahydro‐1H‐3‐benzazepine and 2,3,4,5‐tetrahydro‐1H‐naphth[1,2‐d] azepine derivatives
Authors: Bobowski George , Gottlieb Jeffrey M. , West Barbara , Shavel John
Published: April 2009

The multi‐step synthetic procedures to prepare a number of 2,3,4,5‐tetrahydro‐1H‐benzazepine derivatives 1 through a series of intermediates are described. The condensation of arylaldehydes2with 2‐nitropropanes3gave nitroalcohols4which were reduced to alcohol amines5. The condensation of5with arylacetaldehydes6gave imino derivatives7which on reduction with borohydride gave secondary amines8. By employing different methods, alcohol amines5were condensed with arylacetic acids9to give amides10which were then reduced to amines8. On treatment with mineral acids, amines8were cyclized to the target compounds1. Biological activities of1are also briefly discussed.
Pyridinethiones. IX preparation of ricinidine, thioricinidine and other 2(1H)‐pyridones and ‐thiones related to nicotinic acid
Authors: Becher Jan , Johansen Tea , Michael Maged Aziz
Published: April 2009

2(1H)‐Pyridones and ‐thiones related to 1‐substituted nicotinic acid derivatives have been prepared via the corresponding l‐substituted‐3‐formyl‐2(1H)‐pyridones and ‐thiones. A number of synthetic procedures for the interconversion of functional groups in these nicotinic acid derivatives are given i.e. preparation of the aldoximes, nitriles, carboxamides and carboxylic acids as well as the 3‐ hydroxyalkyl derivatives. The course of the basic peroxide oxidation of the l‐substituted‐3‐formyl‐2(1H)‐pyridinethiones is found to be very dependent upon the electronegativity of the 1‐substituent. A preparation of ricinidine is also described.
An investigation of some base induced transformations of the 1,4‐benzodioxan ring system
Authors: Chapleo Christopher B. , Davis John A. , Myers Peter L. , Readhead Michael J. , Stillings Michael R. , Welbourn Anthony P. , Hampson Frank C. , Sugden Keith
Published: April 2009

The reaction between benzodioxan‐2‐carboxylic acid and ethylenediamine has been examined and related base induced transformations investigated.
The preparation and the nucleophilic reaction of 3,3‐di(1‐azolyl)‐2‐alken‐1‐ones, precursor of acetylketene derivatives
Authors: Kashima Choji , Tajima Tadakuni , Omote And Yoshimori
Published: April 2009

2‐Alken‐1‐ones, 3,3‐di‐(1‐azolyl)‐2‐alken‐1‐ones and related compounds were prepared by two methods. These compounds were found to be the useful precursors for acylketene derivatives such as ketene dithioacetals and diaminals by treatment with various nucleophiles.
The assignment of the 1H‐NMR and 13C‐NMR spectra of 5H‐dibenz[b,f]azepine and 10,11‐dihydro‐5H‐dibenz[b,f]azepine
Authors: Hallberg A. , Al‐Showaier I. , Martin A. R.
Published: April 2009

The total assignments of the 1H‐nmr and 13C‐nmr spectra of 5H‐dibenz[b,f]azepine [1] and 10,11‐dihydro‐5H‐dibenz[b,f]azepine (2) have been made based on comparison with the corresponding 4,6‐dideuterated derivatives 3, and 4. These compounds were prepared via repeated lithiations and subsequent deuterations of 1 and 2.
Synthesis of some 4H,10H[1]benzoxepino[3,4‐c]pyrazol‐4‐one derivatives
Authors: Deshayes Christian , Chabannet Michel , Gelin Suzanne
Published: April 2009

1H(or 2H)4H10H[1]Benzoxepino[3,4‐c]pyrazol‐4‐ones were prepared from phenoxymethylpyrazolecarboxylic acids which in turn were synthesized from simple starting materials. Different pathways to allow the predominant formation of the N‐1 or N‐2 substituted derivatives are described. The isomeric 1 or 2‐substituted structures were supported by 13C‐nmr.
C(6)N(7)‐cyclized purines
Authors: Griengl H. , Hayden W. , Plessing A.
Published: April 2009

By reaction of 6‐[N‐(2‐hydroxyethyl)‐N‐methyl]aminopurine (2a) and of the corresponding 3‐hydroxypropyl derivative 2b with thionyl chloride a bridge to N(1) is formed yielding 5 and 6, respectively, whereas from 6‐[N‐(4‐hydroxybutyl)‐N‐methyl]aminopurine (2c) the 4‐chlorobutyl compound 4 is obtained, which cyclizes in alkaline medium to the C(6)‐N(7) bridged compound 7. A related cyclization to 11a–11f is observed when 6‐chloropurines are reacted with 3‐alkyl‐1,3‐oxazolidines or 3‐methyl‐1,3‐thiazolidine.
Synthesis of bis(2‐chloroethyl)amino‐1,8‐naphthyridines for evaluation as anticancer agents
Authors: Ferrarini Pier Luigi , Mori Claudio , Biagi Giuliana , Livi Oreste , Tonetti Imperio
Published: April 2009

Some 1,8‐naphthyridine nitrogen mustards have been synthesized for studies of their antitumor potentialities. All the tested intermediate and target compounds are devoid of antitumor properties.
Synthesis of some spin‐labeled bithiazoles, Useful probes for studying bleomycin‐DNA binding
Authors: Houssin Raymond , Bernier Jean‐Luc , Hénichart Jean‐Pierre
Published: April 2009

The antibiotic antitumor drug Bleomycin is known to bind to DNA by intercalation of its bithiazole chromophore into the DNA base‐pairs. Four spin‐labeled bithiazoles, bearing a 4‐(2,2,6,6‐tetramethyl‐1‐piperidinooxy) free radical, have been synthesized. These derivatives where the nitroxide group is linked to the end of spacers of various lengths, can be used as probes for the study, by esr spectroscopy, of the intercalation of the heterocyclic moiety of Bleomycin.
Etude de quelques dérivés N‐3‐substitués et N‐1,N‐3‐disubstitués de la cyclohexanospirohydantoîne
Authors: Pedregal Carmen , Trigo Gregorio G. , Espada Modesta , Elguero José , Vincent Emile‐Jean , Faure Robert
Published: April 2009

l'alcoylation de la cyclohexanospirohydantoîne dans des conditions classiques et en transfert de phase conduit respectivement aux derivés N‐3‐substitués et aux derivés N‐1,N‐3‐disubstitués. l'application successive de ces méthodes a permis d'accéder facilement aux hydantoînes portant deux substituants différents. Les différents produits obtenus ont été etudiés par rmn du 13C. Cette méthode permet d'identifier les produits mono‐ et disubstitués ainsi que de déterminer la position du substituant.
Ba(SCN)2(H2O) complex of the cis‐syn‐cis isomer of 2,5,8,15,18,21‐hexaoxatricyclo[20,4,0,09,14]hexacosane(dicyclohexyl‐18‐crown‐6) [Ba(SCN)2(H2O)(C20H36O6)]
Authors: Dalley N. Kent , Sypherd Dirk , George Rose D.
Published: April 2009

The structure of the title compound has been redetermined. Hydrogenation of dibenzo‐18‐crown‐6 yields two conformational isomers which were proposed to be the cis‐syn‐cis and the cis‐trans‐cis isomers of dicyclohexyl‐18‐crown‐6. The previous study had established that the title complex contains the ligand which has the cis‐syn‐cis conformation but had resulted in some inaccurate bond lengths and also in an uncertainty regarding the presence of a water of hydration in the crystal. This study confirmed the report of the general conformation of the complex, resulted in more precise bond lengths and clearly established that a water of hydration was present at the crystal.
Angular heterocycles. A convenient synthesis of 6‐N‐(acetylanilino)‐5H‐benzo[a]phenothiazin‐5‐one, 6‐N‐(acetylanilino)‐5H‐benzo[a]phenoxazin‐5‐ones and their derivatives
Authors: Agarwal N. L. , Ghosh S. , Tripathi A. K. , Atal C. K.
Published: April 2009

The reaction of 2‐N‐(acetylanilino)‐3‐chloro‐1,4‐naphthoquinone (2) with bifunctional aromatic amines afforded angular heterocycles 6 and 7. Reductive acetylation of 7 provided o‐acyl 9 and O,N‐diacyl 10 derivatives depending upon the reaction conditions. The ir, uv, pmr and mass spectral data are also presented.
Methylpyridylbenz‐X‐azoles. lH NMR Study
Authors: Carpignano Rosarina , Savarino Piero , Barni Ermanno , Viscardi Guido
Published: April 2009

The shielding parameters of benz‐X‐azolyl substituents in various positions of the pyridine nucleus were determined by means of a regression analysis procedure. Analogously the shielding contributions of pyridyl substituents on homocyclic protons of benz‐X‐azoles were derived. The results evidence some interactions between the two heterocyclic systems when the benz‐X‐azolyl substituents are linked at the pyridine α‐position.
Mass fragmentation pattern of N‐ and O‐substituted 2‐morpholinols
Authors: Simonotti Luca , Pasqualucci Carmine , Pifferi Giorgio
Published: April 2009

The mass spectra of a series of N‐ and O‐substituted 2‐morpholinols were considered and the complex fragmentation pattern explained on the basis of evidences reported in the literature and of experimental data (high resolution, metastable ions). The primary fragmentations are given by inductive cleavage due to the heteroatoms, while ring contractions, through retro Diels‐Alder reactions, form most of the secondary pattern with different ions related to N‐ and O‐substituents. Moreover, hemiacetals in the tautomeric hydroxyaldehyde form undergo an α‐cleavage.
Phase transfer catalysis in N‐alkylation of the pharmaceutical intermediates phenothiazine and 2‐chlorophenothiazine
Authors: Gozlan Igal , Ladkani David , Halpern Mark , Rabinovitz Mordecai , Avnir David
Published: April 2009

The N‐alkylation of the two title compounds was studied, utilizing phase transfer catalysis (PTC) methods. Very mild reaction conditions were developed, especially for three‐carbon N‐alkylation. Of special interest is the high‐yield synthesis of N‐(3‐chloropropyl)‐2‐chlorophenothiazine. The results are discussed in terms of the classical PTC/OH− mechanisms.
1,2,4‐Triazines. 8. Reduction of 4‐methyl‐1,2,4‐triazin‐5(4H)‐ones with sodium borohydride. Regioselective preparation of dihydro‐1,2,4‐triazin‐5(4H)‐ones
Authors: Sanemitsu Yuzuru , Nakayama Yoshinori , Mizutani Masato , Oshie Kazuyuki
Published: April 2009

Reduction of 3‐methylthio‐1,2,4‐triazin‐5(4H)‐one (1a) with sodium borohydride afforded 3‐methylthio‐1,6‐dihydrotriazin‐5(4H)‐one (2b) selectively. 3‐Methylthio‐6‐t‐butyl‐1,2,4‐triazin‐5(4H)‐one (1d) reacted with sodium borohydride to give mainly 6‐t‐butyl‐2,3‐dihydro‐1,2,4‐triazin‐5(4H)‐one (3d). The reaction of various 4‐methyl‐1,2,4‐triazin‐5(4H)‐ones with sodium borohydride and the influence of bulkiness and electronic effect of the substituents at the 3‐ and 6‐positions upon the product ratio, are also discussed.
Synthesis and properties of 3‐chloro‐ and 3,7‐dichloro‐3,4‐dihydro‐1‐hydroxycarbostyrils and related heterocyclic compounds
Authors: McCord T. J. , DuBose C. E. , Shafer P. L. , Davis A. L.
Published: April 2009

3‐Chloro‐ and 3,7‐dichloro‐3,4‐dihydro‐1‐hydroxycarbostyrils were synthesized by the catalytic hydrogenation of the α‐chloro‐ and α,4‐dichloro‐β‐(o‐nitrophenyl)propionic acids in strong acidic solution over platinum‐on‐carbon sulfided catalyst. However, the catalytic hydrogenation of α‐bromo‐β‐(o‐nitrophenyl)propionic acid yielded 3,4‐dihydro‐1‐hydroxycarbostyril under the same experimental conditions. The 3‐chloro‐3,4‐dihydro‐1‐hydroxycarbostyril and the α‐chloro‐β‐(o‐nitrophenyl)propionic acid underwent facile dehydrochlorination in mild alkaline solution to give 1‐hydroxycarbostyril and o‐nitrocinnamic acid, respectively. Selective reduction of 3‐chloro‐3,4‐dihydro‐1‐hydroxycarbostyril and 1‐hydroxycarbostyril to the corresponding lactams, 3‐chloro‐3,4‐dihydrocarbostyril and carbostyril, was effected by catalytic hydrogenation in hydrochloric acid over platinum black catalyst. The structures of the substituted carbostyril derivatives were correlated with their proton nmr spectra.
A short synthesis of 2H‐1‐benzopyrans
Authors: Schuda Paul Francis , Phillips Jennifer L.
Published: April 2009

A two‐step process for synthesizing 2H‐1‐benzopyrans from phenols and β‐halopropionaldehyde acetals is detailed.
Synthesis of fluorinated pyridines by the balz‐schiemann reaction. An alternative route to enoxacin, a new antibacterial pyridonecarboxylic acid
Authors: Matsumoto Jun‐Ichi , Miyamoto Teruyuki , Minamida Akira , Nishimura Yoshiro , Egawa Hiroshi , Nishimura Haruki
Published: April 2009

Fluorination of the 2,6‐disubstituted 3‐aminopyridines 5 and 12 by the Balz‐Schiemann reaction is described. 2,6‐Dichloro‐3‐pyridinediazonium tetrafluoroborate (6) and 2‐substituted 6‐acetylamino‐3‐pyridinediazonium tetrafluoroborates 13 were heated with or without a solvent to give the corresponding fluorinated pyridines 7 and 14, respectively, in good yields. 2‐Substituted 6‐acetylamino‐3‐fluoropyridines (14) were converted by a known method into a series of 7‐substituted 1‐ethyl‐6‐fluoro‐1,4‐dihydro‐4‐oxo‐1,8‐naphthyridine‐3‐carboxylic acids 21 including enoxacin [1‐ethyl‐6‐fluoro‐1,4‐dihydro‐4‐oxo‐7‐(1‐piperazinyl)‐1,8‐naphthyridine‐3‐carboxylic acid [(2)], a new potential antibacterial agent.
Aminoalkyl derivatives of 2,4′‐bithiazole‐4‐carboxylic acid, the intercalating part of bleomycin
Authors: Houssin Raymond , Bernier Jean‐Luc , Hénichart Jean‐Pierre
Published: April 2009

The synthesis of three 2,4′‐bithiazole derivatives related to the antibiotic antitumor bleomycin is reported. These compounds substituted by aminoalkyl chains on 2′ and/or 4‐positions were prepared by the Hantzs synthesis between new thioamides and methyl 2‐(2‐bromoacetyl)thiazole‐4‐carboxylate and will be useful for the study of the intercalative moiety of bleomycin.
The synthesis of substituted pyrido[1′,2′:1,5]pyrazolo[3,4‐d]pyrimidines
Authors: Molina P. , Arques A. , Hernandez H.
Published: April 2009

A convenient synthesis of derivatives of the pyrido[1′,2′:1,5]pyrazolo[3,4‐d]pyrimidine ring system from readily available 2‐amino‐3‐cyano‐5,7‐diphenylpyrazolo[1,5‐a]pyridine I and carbon disulfide, aryl isothiocyanates or nitriles is described. Derivatives of compound I undergo cyclization to the titled ring system by action of dimethylformamide dimethylacetal or hydrogen sulfide followed by treatment with triethylamine.
Synthesis of 1,3,4‐oxadiazaspiro[4.4]nona‐2,6,8‐trienes via 1,3‐dipolar cycloadditions of diphenylnitrilimine with cyclopentadienones. Crystal and molecular structure of a cycloadduct
Authors: Tsatsaroni E. G. , Argyropoulos N. G. , Alexandrou N. E. , Houndas A. , Terzis A.
Published: April 2009

The cycloaddition of diphenylnitrilimine with substituted cyclopentadienones leads to the formation of the title spirooxadiazoline derivatives 2, in good yields. The reaction is examined on the basis of the frontier molecular orbitals of the reacting reagents. An X‐ray crystallographic analysis of the product 2b is made.
The synthesis of lin‐benzoreumycin, lin‐benzo‐1‐methylxanthine, and lin‐benzo‐1,9‐dimethylxanthine
Authors: Schneller Stewart W. , Ibay Augusto C. , Christ William J.
Published: April 2009

Commencing with 7‐chloro‐3‐methylquinazoline‐2,4(1H,3H)‐dione (9a), a five step synthesis of 7‐methylpyrimido[5,4‐g]‐1,2,4‐benzotriazine‐6,8(7H,9H)‐dione (lin‐benzoreumycin, 6) has been accomplished. A synthesis of 1,7‐dimethylpyrimido[5,4‐g]‐1,2,4‐benzotriazine‐6,8(1H,7H)‐dione (lin‐benzotoxoflavin, 5) employing an intermediate from the preparation of 6 (i.e., 7‐chloro‐3‐methyl‐6‐nitroquinazoline‐2,4(1H,3H)‐dione, 9b) was attempted but could not be accomplished beyond the dihydro precursor of 5 (i.e., 12). Compound 9b did lead to successful preparations of 7‐methylimidazo[4,5‐g]quinazoline‐6,8(5H,7H)‐dione (lin‐benzo‐1‐methylxanthine, 7) and 3,7‐dimethylimidazo[4,5‐g]quinazoline‐6,8(5H,7H)‐dione (lin‐benzo‐1,9‐dimethylxanthine, 8) by first reacting 9b with ammonia (for 7) or methylamine (for 8) followed by reductive cyclization in formic acid.
Mass spectral fragmentation patterns of heterocycles. VI. Carbazole and 1,8‐dideuteriocarbazole
Authors: Hallberg Anders , Martin Arnold R.
Published: April 2009

The mass spectral fragmentation of carbazole was reinvestigated using metastable ion studies, exact mass measurements and 1,8‐dideuteriocarbazole. 1,8‐Dideuteriocarbazole was prepared by successive metalations and deuterations of carbazole. The 1H‐ and 13C‐nmr spectra of 1,8‐dideuteriocarbazole confirmed earlier assignments for carbazole.
The reaction of substituted thiosemicarbazides and γ‐haloketones
Authors: Jones Winton D. , Kane John M. , Sill Arthur D.
Published: April 2009

The reactions of substituted thiosemicarbazides and γ‐halobutyrophenones afforded derivatives of the tetrahydro‐1H‐pyrrolo[1,2‐b][1,2,4]triazole‐2(3H)‐thione ring system.
N2′‐acetyl‐6‐diacetoxymethylpterin
Authors: Boyle Peter H. , O'Mahony Mary J.
Published: April 2009

Treatment of folic acid with bromine in 48% hydrobromic acid gives the hydrobromide salt of 6‐formylpterin (1), and acetylation of 1 with recovered acetic anhydride leads to N2′‐acetyl‐6‐diacetoxymethylpterin (3).
Reaction of 2‐hydrazinoperimidine with acetylacetone
Authors: Liu Kang‐Chien , Chen Hsiu‐Ho
Published: April 2009

Heating 2‐hydrazinoperimidine (2) with acetylacetone in absolute ethanol gave exclusively 2‐(3,5‐dimethyl‐1‐pyrazolyl)perimidine (4) via a [2 + 3] cyclization. The possible [4 + 3] condensate, 3,5‐dimethyl‐1H‐1,2,4‐triazepino[4,3‐a]perimidine (5) was not produced. Spectral analyses were applied to the structure elucidation of the products.
The chemistry of 2H‐3,1‐benzoxazine‐2,4(1H)‐dione (isatoic anhydride). 14. A facile entry into the acronycine ring system
Authors: Coppola Gary M.
Published: April 2009

6‐Demethoxyacronycine (9), containing the acronycine nucleus, has been readily synthesized in two steps via the reaction of N‐methylisatoic anhydride with the enolate derived from 2,6,7,8‐tetrahydro‐2,2‐dimethyl‐5H‐1‐benzopyran‐5‐one (8) followed by oxidation with DDQ.
Reaction of 2‐acyl‐3‐aminobenzofurans with hydrazines
Authors: Gatta Franco , Settimj Guido
Published: April 2009

While 2‐acetyl and 2‐benzoyl‐3‐aminobenzofurans did not react with hydrazine, monomethyl‐ and N,N‐dimethylhydrazine to give the related hydrazones, their 3‐N‐(p‐toluenesulfonyl) derivatives afforded them smoothly in good yields. Depending upon reaction conditions, products arising from hydrazone cyclization to benzofuropyrazoles and/or from furan ring cleavage at the C2O bond to give 5‐(2‐hydroxyphenyl)pyrazoles were also formed. The formation of these products depends upon hydrazones configuration and is discussed. Only (E)‐isomers appear to undergo furan ring opening. In acidic media at room temprature either the hydrazones or the monomethylhydrazones gave the same related α‐azines. Microanalyses, ir, uv, 1H‐nmr and ms spectra are in agreement with the proposed structures.
Reactions with 5‐aminopyrazoles. I. Synthesis of halogen‐containing fused pyrazoles
Authors: Hammouda Hamdy A. , El‐Barbary Ahmed A. , Sharaf Mohie A. F.
Published: April 2009

5‐Amino‐3‐phenylpyrazole (I) and 5‐amino‐4‐bromo‐3‐phenylpyrazole (II) reacted with ethyl acetoacetate and acetylacetone to give various pyrazolo[1,5‐a]pyrimidines IV‐VI and with benzoins to give different fused pyrazoles, namely, imidazo[1,2‐b]pyrazoles IX, pyrrolo[2,3‐c]pyrazoles X and pyrazolo[4,3‐b][1,4]oxazines XII. Diazotized II was coupled with active methylene‐containing nitriles to afford pyrazolo[5,1‐c]‐as‐triazines XIV.
Studies in spiroheterocycles. Part V. Synthesis of new fluorinated spiro[3H‐indole‐3,2′‐oxiran]‐2(1H)‐ones
Authors: Joshi Krishna C. , Jain Renuka , Garg Saroj
Published: April 2009

Reinvestigation of the reaction of 3‐aroylmethyleneindol‐2‐ones with hydrogen peroxide has revealed that a 1:1 isomeric mixture of spiro[3H‐indole‐3,2′‐oxiran]‐2(1H)‐ones is formed. The structures of the two isomers have been confirmed by their ir, pmr and mass spectral studies. Mass fragmentation patterns of these compounds are discussed.
Photosensitized oxidation of furans. X. Solvent effect in the nuclear magnetic resonance of functionalized diacyloxiranes
Authors: Graziano M. L. , Mayol L.
Published: April 2009

A simple, rapid method to determine the configuration of 2‐alkoxycarbonyl‐2,3‐diacyloxiranes and 2‐alkoxycarbonyl‐2,3‐diacyl‐3‐methyloxiranes is described. The method is based on the observation of the solvent effect on the chemical shifts of the proton or the methyl group linked to the oxirane ring.
Synthesis of some pyrazolo[4,3‐e][1,2]‐ and thiazolo[4,5‐e][1,2]thiazine 1,1‐dioxide derivatives
Authors: Bellemin Robert , Festal Didier
Published: April 2009

The synthesis of various 2‐methylpyrazolo[4,3‐e]‐ and thiazolo[4,5‐e][1,2]thiazine 1,1‐dioxide derivatives is described.
Synthesis of isoquinobenzodiazepinediones
Authors: GÁll‐IstÓk KlÁra , Sterk Lili , TÓth GÁbor , Deák Gyula
Published: April 2009

1‐(2′‐Chloroacetylamino)‐4,4‐dimethyl‐1,4‐dihydro‐3(2H)‐isoquinolinone (3) was cyclised by treatment with sodium hydride in dimethyl sulphoxide containing 0.1 % of water to give 10,10‐dimethyl‐6,7,9,10‐tetrahydro‐5H,14bH‐isoquino[2,1‐d][1,4]benzodiazepine‐6,9‐dione (4) in a yield of 80%. In anhydrous dimethyl sulphoxide the main product of the reaction was 5‐N‐(4,4‐dimethyl‐1‐phenyl‐1,4‐dihydro‐3(2H)‐isoquinolinon‐1′‐yl)isoquino[2,1‐d][1,4]benzodiazepine‐6,9‐dione (5), which was also prepared by the reaction of 3 with 4.
Nitrations of acylamino‐ and nitrodibenzo‐p‐dioxins
Authors: Oliver James E.
Published: April 2009

Nitrations of 1‐ or 2‐acylamino (and nitro) dibenzo‐p‐dioxins were employed to achieve regioselective further functionalization of these compounds. The choice of nitrating conditions and/or acyl substituent (CH3CO vs. CF3CO) often dictated into which ring the first nitro goroup was directed. In almost all cases, nitrations at the 2,3,7,8‐positions were highly favored over nitrations at the 1,4,6,9‐positions; with ammonium nitrate/trifluoroacetic anhydride in tetrahydrofuran, however, nitration of 1‐(trifluoroacetylamino)dibenzo‐p‐dioxin proceeded predominantly at the 4‐position.
v‐Triazolines. Part XIX. Thiocino[4,5‐d]‐1,2,3‐triazole and thiocino[4,5‐d]isoxazole derivatives
Authors: Almirante Nicoletta , Forti Luciana
Published: April 2009

5‐Amino‐2,3,6,7‐tetrahydrothiocines were reacted with arylazides yielding 1‐aryl‐9a‐amino‐1,3a,4,5,7,8,9,9a‐octahydrothiocino[4,5‐d]‐1,2,3‐triazoles which could be deaminated to 1‐aryl‐1,4,5,7,8,9‐hexahydrothiocino‐[4,5‐d]‐1,2,3‐triazoles. Similarly, the above enamines yielded, with nitrile oxides, 3‐aryl‐9a‐amino‐3a,4,5,8,9,9a‐hexahydrothiocino[4,5‐d]isoxazoles which were transformed with acids into 3‐aril‐4,5,8,9‐tetrahydrothiocino‐[4,5‐d]isoxazoles.
The stereochemistry of 4,8‐dimethyl‐6‐phenyl‐5,6,7,8‐tetrahydro‐4H‐1,3,6‐dioxazocin‐2‐ones using NMR
Authors: Nishiyama Tomihiro , Ikemoto Etsuo , Yamada Fukiko
Published: April 2009

Two isomeric 4,8‐dimethyl‐6‐phenyl‐5,6,7,8‐tetrahydro‐4H‐1,3,6‐dioxazocin‐2‐ones were prepared, and their pmr and cmr spectra were examined. From the tris(dipivaloylmethanato) europium (Eu(dpm)3) shift reagent and the dihedral angle, the title compounds are found to exist in the eq‐ax and eq‐eq methyl groups with boat‐chair form.
Stereochemical assignments of the 6‐phenyl‐2‐oxabicyclo[3.1.0]hexanes
Authors: Schaub Lowry P. , Woodyard James D.
Published: April 2009

Preparation and stereochemical assignments of the 6‐phenyl‐2‐oxabicyclo[3.1.0]hexanes are reported. The stereochemical assignments are based on chemical as well as nmr data.
Synthesis of some new mesoionic heterocycles
Authors: Taneja Vineeta , Anand Madhu , Gupta C. L. , Gupta S. B. , Mital R. L.
Published: April 2009

The synthesis of various substituted 1‐hydroxy‐2‐chloroacetyl‐6‐thia‐10b‐aza‐2a‐azoniaaceanthrylene hydroxide inner salt, 1‐hydroxy‐6‐thia‐10b‐aza‐2a‐azoniaaceanthrylene hydroxide inner salt, 1‐hydroxy‐2‐piperidinoacetyl‐6‐thia‐10b‐aza‐2a‐azoniaaceanthrylene hydroxide inner salt is described. The ir is also included.
The reactivity of 4‐hydroxy‐6‐methyl‐2‐pyrone towards different types of ketones
Authors: De March P. , Roca J. L. , Moreno‐Mañas M. , Pleixats R.
Published: April 2009

4‐Hydroxy‐6‐methyl‐2‐pyrone (triacetic acid lactone) reacts at C‐3 with acetone, mesityl oxide and pentane‐2,4‐dione. The structures of the final products have been elucidated.
Reactions of 1,3‐thiazine‐2,6‐dithiones. Part 5. Novel synthesis of 3,5‐dicyano‐4‐thiopyridones via 2‐cyanomethyldihydro‐1,3‐thiazine‐6‐thiones
Authors: Muraoka Motomu , Yamamoto Tatsuo
Published: April 2009

A novel synthesis of a series of 2,6‐disubstituted 3,5‐dicyano‐4‐thiopyridones 4 by the decomposition of 2,4‐disubstituted 5‐cyano‐2‐cyanomethyldihydro‐1,3‐thiazine‐6‐thiones 2, which are synthesized from 4‐substituted 5‐cyano‐1,3‐thiazine‐2,6‐dithiones and enaminonitriles, is described.
Derivatives of benzo[4,5]cyclohepta[1,2‐b]thiophene 3. Synthesis of 2,3,6,7‐tetrahydro‐3‐oxobenzo[1,2]cyclohepta[3,4,5‐hi]thieno[3,4‐c]pyridine and 2,3,7,8‐tetrahydro‐3‐oxothieno[2,1‐b]cyclohepta[5,6,7‐de]isoquinoline
Authors: Arribas Enrique , Vega Salvador
Published: April 2009

The title compounds 3 and 4 were synthesized by cyclization via isocyanate of the Z and E‐9,10‐dihydro‐4H‐benzo[4,5]cyclohepta[1,2‐b]thiophene‐4‐ylidenacetic acids 8 and 9, which in turn were prepared by the Wadsworth‐Emmons reaction of ketone 5 with triethyl phosphonacetate followed by separation and independent hydrolysis of the corresponding esters 6 and 7. The structures of these new compounds as well as the configurations of their isomeric precursors are described.
13C NMR spectral assignments of chlorpromazine and its 5‐oxide. Literature correction
Authors: Jovanovic Misa V. , Biehl E. R.
Published: April 2009

The 13C chemical shift assignments of title compounds were made on the basis of their coupled and decoupled spectra. The size of the ipso and allylic 13CH coupling constants establish unequivocally the identity of symmetry related carbon pairs and show that several assignments reported previously are incorrect.
Reaction of chlorosulfonyl isocyanate with aziridines
Authors: Murthy K. S. Keshava , Dhar D. N.
Published: April 2009

The reaction of chlorosulfonyl isocyanate (CSI) with 1,2,3‐triphenylaziridine (1) and some cis‐ and trans‐1‐cyclohexyl‐2‐aroyl‐3‐phenylaziridines, 4‐7 and 19‐22 has been described. The cis‐isomers of aziridines, 4‐7, undergo a smooth reaction with CSI to give the corresponding cis‐isomers of 2‐chlorosulfonylimino‐1,3‐oxazolidines, 8‐11, in good yields (65‐67%). While the trans‐isomers, 19‐22, gave unusual products 23‐26 which have been assigned a bicyclic structure, based on their physical and spectral (ir, pmr, ms) data. Plausible mechanisms have been postulated to explain the transformations.
Functionalization of substituted 2(1H)‐pyridones. V. The synthesis of 1,2‐dihydro‐2‐oxo‐3,5‐pyridinedicarboxylic acid derivatives through a novel dianion route
Authors: Domagala John M.
Published: April 2009

A new pyridone dianion was prepared by halogen‐metal exchange from 5‐bromo‐1,2‐dihydro‐2‐oxo‐3‐pyrid‐inecarboxylic acid, t‐butyl ester and two equivalents of n‐butyllithium. This 1,5‐dianion readily reacted at C5 with electrophiles. Quenching with carbon dioxide gave the previously unreported 1,2‐dihydro‐2‐oxo‐3,5‐pyridine dicarboxylic acid, 3‐t‐butyl ester. The 5‐carboxyl groups were selectively converted to the ethyl ester and the ethyl amide through the 5‐imidazolide. The 3‐t‐butyl ester was easily removed from all derivatives with acid hydrolysis.
The synthesis of some derivatives of benzo[f]naphtho[1,8‐bc]thiepin‐12‐one
Authors: Flores Maria Celia , Beller Nicholas R. , Castrillón JosÉ
Published: April 2009

The preparations of benzo[f]naphtho[1,8‐bc]thiepin‐12‐one, its 6‐methyl and 6‐methoxy derivatives and their corresponding sulfoxides and sulfones are described. They involve the coupling of suitable halogen naphthyl derivatives with thiophenoxides with the help of copper and the cyclization of the resulting acids with phosphorus pentoxide in benzene. The oxidations to sulfoxides and sulfones were performed with iodo‐benzene diacetate and hydrogen peroxide, respectively. The ir and pmr spectra are reported.
Synthèse de dérivés du tétrathiafulvalène à propriétés mésomorphogènes
Authors: Polycarpe Catherine , Torreilles Eliane , Giral Louis , Babeau Annick , Tinh Nguyen‐Hun , Gasparoux Henri
Published: April 2009

Nous décrivons la synthèse de bis (alkyl‐4 phényl) et bis (alkoxy‐4 phényl) tétrathiafulvalènes originaux. Certains d'entre eux présentent un polymorphisme dont on a précisé les températures de transition.
The synthesis of propellance compounds from 2,3‐disubsituted indoles and o‐benzoquinones
Authors: Omote Yoshimori , Harada Kazuo , Tomotake Atsushi , Kashima Choji
Published: April 2009

The reaction of 2,3‐dihydro‐1H‐cyclopent[b]indole 3 and 1,2,3,4‐tetrahydrocarbazole 4 with substituted o‐benzoquinones yielded [4.3.3]‐ and [4.4.3]propellanes, respectively. The physical and chemical properties of the propellane compounds were investigated and a mechanism for the formation of the propellane compounds was discussed.
Twice wind onsets of monsoon over the western North Pacific and their simulations in AMIP models
Authors: Zhang Li , Li Jianping
Published: April 2009

The absolute angle between wind vectors is used to investigate and describe the seasonal evolutions of wind direction, which is able to indicate the abrupt seasonal shift and stable seasonal state of winds. The results show that the wind directions over the western North Pacific (WNP, 10° –22.5°N, 125° –145°E) undergo two abrupt changes and three stable states from winter to summer. Here we name the phenomenon as twice wind onsets of monsoon. The first wind onset occurs near mid‐May at 15°N, and the second one happens with the wind direction shifting southwesterly in mid‐July and ends in late September. The variations of Outgoing Longwave Radiation (OLR) and rainfall in the northward 5° latitudes of the neighbouring region show similar abrupt features as those of the twice wind onsets. The western Pacific subtropical high (WPSH) retreats eastward in the second stable state (pentad 29 to 37), which differs from the first stable state (pentad 1 to 24). As the strong cross‐equator flows from the Southern Hemisphere reach the WNP, the eastward retreat of WPSH consequently triggers the first wind onset. Then the WPSH ridge suddenly jumps to 30°N and results in the second wind onset. Meanwhile, the propagation of the second wind onset is consistent with the migration of the WNP monsoon trough.

Seven atmospheric general circulation models (AGCMs) of Atmospheric Model Intercomparison Project (AMIP) from Intergovernmental Panel on Climate Change (IPCC) Fourth Assessment Report (AR4) are validated against the observations mentioned earlier. The results show that there are still notable shortcomings for the models to simulate the WNP summer monsoon, especially the twice onsets. There is no significant improvement for the simulation of multi‐models ensemble mean. Only MPI‐ECHAM5 captures partial characteristics of similar pattern. The poor simulation of the migration of the WPSH ridge and monsoon trough may be important factors for the shortcomings. Moreover, none of the models reproduces corresponding rainfall patterns over the WNP. Copyright © 2009 Royal Meteorological Society
Raman spectroscopic study of synthetic reevesite and cobalt substituted reevesite (Ni,Co)6Fe2(OH)16(CO3)·4H2O
Authors: Frost Ray L. , Bakon Kathleen H. , Palmer Sara J.
Published: April 2009

Raman spectroscopy, complemented with infrared spectroscopy of compounds equivalent to reevesite, formula (Ni,Co)6Fe2(OH)16(CO3)·4H2O, with the ratio of Ni/Co ranging from 0 to 1, have been synthesised and characterised based on the molecular structure of the synthesised mineral. The combination of Raman spectroscopy with infrared spectroscopy enables an assessment of bands attributable to water stretching and brucite‐like surface hydroxyl units to be obtained. Raman spectroscopy shows a reduction in the symmetry of the carbonate anion, leading to the conclusion that the carbonate anion is bonded to the brucite‐like hydroxyl surface and to the water in the interlayer. Variation in the position of the carbonate anion stretching vibrations occurs and is dependent on the Ni/Co ratio. Water bending modes are identified in both the Raman and infrared spectra at positions greater than 1620 cm−1, indicating that water is strongly hydrogen bonded to both the interlayer anions and the hydrotalcite surface. Copyright © 2009 John Wiley & Sons, Ltd.
Surface‐enhanced Raman scattering of 4‐mercaptopyridine on sub‐monolayers of α‐Fe2O3 nanocrystals (sphere, spindle, cube)
Authors: Fu Xiaoqi , Bei Fengli , Wang Xin , Yang Xujie , Lu Lude
Published: April 2009

We report surface‐enhanced Raman scattering (SERS) spectra from 4‐mercaptopyridine (4‐Mpy) adsorbed on sub‐monolayers of α‐Fe2O3 nanocrystals (sphere, spindle, cube). The maximum enhancement factor has been estimated to be about 104 compared to that of 4‐Mpy in solution. A possible mechanism has been proposed that the charge transfer between the α‐Fe2O3 nanocrystals and the 4‐Mpy molecules is most likely responsible for the observed enhancement of Raman intensity of adsorbed 4‐Mpy molecules as surface plasmon resonances have not occurred. Copyright © 2009 John Wiley & Sons, Ltd.
Impact of newborn hearing screening
Authors: Philips Birgit , Corthals Paul , De Raeve Leo , D'haenens Wendy , Maes Leen , Bockstael Annelies , Keppler Hannah , Swinnen Freya , De Vel Eddy , Vinck Bart , Dhooge Ingeborg
Published: April 2009

Objectives/Hypothesis:

To evaluate the impact of a newborn hearing screening program on the management and outcome of deaf children and to identify underlying factors that may be responsible for the differences between high and low performing implanted children.

Study Design:

Retrospective cohort study of 391 implanted children in Flanders (Belgium).

Methods:

First, implanted children were sorted into two groups on account of screening age (early screened, n = 195 vs. late screened, n = 196). Both groups were compared with respect to several variables. Second, outcome of cochlear implantation was measured in terms of the child's speech perception and production skills (n = 355). A subgroup of high performing cochlear implant (CI) users was compared with low performing CI users with regard to several variables.

Results:

Early screened children differ significantly from late screened children with respect to age of hearing loss detection and age at cochlear implantation. Furthermore, early screening and implantation is associated with better auditory receptive skills and speech intelligibility. Additional impairments negatively influence both receptive and productive skills. In addition, children who communicate orally and wear bilateral cochlear implants perform better on speech production, whereas a better speech perception was found in children who became progressively deaf as opposed to congenitally deaf children.

Conclusions:

The results of this extensive study of profoundly deaf children with CIs in Flanders indicate that a newborn hearing screening program results in earlier intervention in deaf children, which beneficially influences the auditory receptive skills and speech intelligibility. Laryngoscope, 2009
Proteomics analysis of perilymph and cerebrospinal fluid in mouse
Authors: Leary Swan Erin E. , Peppi Marcello , Chen Zhiqiang , Green Karin M. , Evans James E. , McKenna Michael J. , Mescher Mark J. , Kujawa Sharon G. , Sewell William F.
Published: April 2009

Objectives:

Proteins in perilymph may alter the delivery profile of implantable intracochlear drug delivery systems through biofouling. Knowledge of protein composition will help anticipate interactions with delivered agents.

Study Design:

Analysis of mouse perilymph.

Methods:

Protein composition of perilymph and cerebrospinal fluid (CSF) was analyzed using a capillary liquid chromatography‐mass spectrometry‐based iTRAQ quantitative proteomics approach. We searched against a mouse subset of the Uniprot FASTA protein database. We sampled perilymph from the apex of the mouse cochlea to minimize CSF contamination.

Results:

More than 50 explicit protein isoforms were identified with very high confidence. iTRAQ reporter ions allowed determination of relative molar amounts of proteins between perilymph and CSF. Protein in perilymph was almost three times more concentrated than in CSF. More than one‐third of the proteins in perilymph comprised protease inhibitors, with serpins being the predominant group. Apolipoproteins constituted 16%. Fifteen percent of the proteins were enzymes. Albumin was the most abundant single protein (14%). Proteins with relatively high perilymph/CSF ratios included broad‐spectrum protease inhibitors and apolipoproteins.

Discussion:

Some proteins found in perilymph, such as albumin and HMW kininogen, have been implicated in biofouling through adsorption to device materials. The relatively large quantities of apolipoprotein and albumin may serve as a reservoir for acidic and lipophillic drugs. Alpha‐2‐glycoprotein can bind basic drugs.

Conclusions:

Perilymph is similar in protein composition to CSF, though amounts are 2.8 times higher. Protease inhibitors comprise the largest category of proteins. Laryngoscope, 2009
A systematic review of outcomes following surgical decompression for dysthyroid orbitopathy
Authors: Leong Samuel C. , Karkos Peter D. , MacEwen Caroline J. , White Paul S.
Published: April 2009

Objectives:

To systematically review and compare the surgical outcomes of orbital decompression for dysthyroid orbitopathy.

Methods:

Data sources used were PubMed, EMBASE, and Cochrane search for English‐language literature from January 1990 to April 2008, combined with manual review of citations within article bibliographies. Citations acquired from the targeted search were filtered independently by two researchers. Relevant articles were reviewed to obtain information including interventions and outcome measures. Articles were then assigned level‐of‐evidence grades as defined by the Oxford Centre for Evidence‐Based Medicine.

Results:

A total of 516 citations were generated from which 135 abstracts were regarded as potentially relevant. After other relevant articles identified from the bibliography and duplicate articles excluded, 56 studies were available for analysis. Fifty studies were identified as level 4 and six as level 3 evidence. A total of 2,315 patients were pooled, from which 4,176 orbits were decompressed. Fifteen different surgical techniques were broadly identified. The most common surgical indication was cosmesis. Decompression by combined transpalpebral‐endoscopic technique resulted in the highest average reduction in postoperative proptosis. The largest improvement in visual acuity was after coronal approach orbital decompression. The overall complication rate was 9.3%. The most significant complications were vision loss and cerebral vascular accident. The highest complication rate was associated with combined endoscopic and transpalpebral decompression.

Conclusions:

There are myriad techniques in practice for decompressing the orbit, but no one technique has yet to achieve consistently good outcome and low complication rates. The reporting of outcomes should conform to a minimum dataset. Laryngoscope, 2009
Investigation on the corrosion inhibitive effect of 2H‐pyrazole‐triazole derivatives in acidic solution
Authors: Li Weihua , Zhao Xia , Liu Faqian , Deng Junying , Hou Baorong
Published: April 2009

Four research methods, such as weight loss test, electrochemical techniques, adsorption isotherm, and quantum chemical calculation, were employed in this paper to study the inhibition efficiency (IE) and inhibition mechanism of three 2H‐pyrazole‐triazole derivatives, BHOT, FHOT, and CHOT in 1 M HCl solution for mild steel. Using the electrochemical technique, three inhibitors were proved to show a mixed‐type character for mild steel by suppressing both anodic and cathodic reactions on the steel surface. The adsorption models of three compounds were established at different temperatures according to their adsorption isotherms. The results of the quantum chemical calculation method indicated that the adsorption sites of 2H‐pyrazole‐triazole derivatives were strongly centralized on benzene ring, triazole ring, or other substituents. All the results showed that the three derivatives were excellent inhibitors in 1 M HCl solution for mild steel.
Glycoproteomics in neurodegenerative diseases
Authors: Hwang Hyejin , Zhang Jianpeng , Chung Kathryn A. , Leverenz James B. , Zabetian Cyrus P. , Peskind Elaine R. , Jankovic Joseph , Su Zhen , Hancock Aneeka M. , Pan Catherine , Montine Thomas J. , Pan Sheng , Nutt John , Albin Roger , Gearing Marla , Beyer Richard P. , Shi Min , Zhang Jing
Published: April 2009

Protein glycosylation regulates protein function and cellular distribution. Additionally, aberrant protein glycosylations have been recognized to play major roles in human disorders, including neurodegenerative diseases. Glycoproteomics, a branch of proteomics that catalogs and quantifies glycoproteins, provides a powerful means to systematically profile the glycopeptides or glycoproteins of a complex mixture that are highly enriched in body fluids, and therefore, carry great potential to be diagnostic and/or prognostic markers. Application of this mass spectrometry‐based technology to the study of neurodegenerative disorders (e.g., Alzheimer's disease and Parkinson's disease) is relatively new, and is expected to provide insight into the biochemical pathogenesis of neurodegeneration, as well as biomarker discovery. In this review, we have summarized the current understanding of glycoproteins in biology and neurodegenerative disease, and have discussed existing proteomic technologies that are utilized to characterize glycoproteins. Some of the ongoing studies, where glycoproteins isolated from cerebrospinal fluid and human brain are being characterized in Parkinson's disease at different stages versus controls, are presented, along with future applications of targeted validation of brain specific glycoproteins in body fluids. © 2009 Wiley Periodicals, Inc., Mass Spec Rev 29:79–125, 2010
Pronation–supination torque and associated electromyographic activity varies during a sustained elbow flexor contraction but does not influence the time to task failure
Authors: Staudenmann Didier , Rudroff Thorsten , Enoka Roger M.
Published: April 2009

In this study we measured the pronation–supination torque, flexion force, and electromyographic activity in elbow flexor muscles during an isometric contraction in which a submaximal elbow flexion force was kept constant for as long as possible. Ten subjects performed the contraction at 20% of maximal voluntary contraction (MVC) torque until failure. Electromyographic (EMG) activity of the long and short heads of biceps brachii, brachialis, brachioradialis, and triceps brachii was recorded with surface and intramuscular electrodes. The mean time to failure was 8.2 ± 6.2 min. The fluctuations in flexion force and pronation–supination torque were correlated (r range = 0.68–0.92), and subjects exhibited a range of pronation–torque profiles that were not associated with the time to failure. Knowing the influence of concurrent actions about the pronation–supination axis during a submaximal fatiguing contraction with the elbow flexor muscles has implications for the design of workstations in ergonomic settings and in the prescription of activities for rehabilitation programs. Muscle Nerve 40: 231–239, 2009