摘要:

AbstractThe crystal and molecular structure of the title compound was determined by single‐crystal x‐ray diffraction techniques. The compound crystallizes in the orthorhombic space group Pca21, with four molecules in a unit cell of dimensions a = 17.552 ± .003, b = 8.235 ± .0008 and c = 11.914 ± .001 Å. The structure was solved by the heavy atom method and refined by full matrix least squares to a final value of R = 0.055 for the 740 independently measured, statistically significant reflections. The conformation of the cyclodecane ring in the bicyclic system differs from the idealized cyclodecane ring based on conformational studies and previous x‐ray determinations of simpler systems. The differences in conformation are

ISSN:0022-152X    

DOI:10.1002/jhet.5570070401

出版商:Wiley‐Blackwell    

年代:1970

数据来源: WILEY

摘要:

AbstractSynthesis of the I‐oxide (2) of the photochromicN‐(3‐pyridyl) sydnone (1), ofN‐(5‐bromo‐3‐pyridyl) sydnone (3), and the I‐oxide (4) of3were undertaken in order to study the effect on photochromism exerted by substituents on the pyridine ring. Compounds2and3were preparedviathe corresponding aminopyridines andN‐pyridylglycines by the general procedure used earlier to prepare1. The required amines, 3‐aminopyridine I‐oxide and 3‐amino‐5‐bromopyridine, were obtained by Hofmann rearrangement of the corresponding amides. An excellent preparation of 5‐bromonicotinamide was developed involving bromination in thionyl chloride followed by reaction of the bromoacid chloride with ammonia in chloroform. Proof of structure for2and3was accomplished by acid hydrolysis to the corresponding hydrazines, which were isolated, respectively, as acetophenone 3‐pyridylhydrazone I‐oxide and as 5‐bromo‐3‐pyridylhydrazine hydrochloride. These products were identical with samples prepared by reduction of the respective diazotized amines. Sydnone4eluded preparation by this general procedure. 3‐Amino‐5‐bromopyridine I‐oxide was prepared conveniently from 5‐bromonicotinamide but attempts to prepare the corresponding glycine by catalytic hydrogenation of a mixture of the amine and butyl glyoxylate afforded, in acid solution,N‐(3‐pyridyl)glycine and, in neutral or alkaline solution, the I‐oxide ofN‐(3‐pyridyl)glycine. Both products resulted from the reductive

ISSN:0022-152X    

DOI:10.1002/jhet.5570070402

出版商:Wiley‐Blackwell    

年代:1970

数据来源: WILEY

摘要:

AbstractA general synthesis of 1,2,4‐triazines, from 3‐methylthiotriazines is described. It has been shown that 1,2,4‐triazines undergo covalent hydration across the N4

ISSN:0022-152X    

DOI:10.1002/jhet.5570070403

出版商:Wiley‐Blackwell    

年代:1970

数据来源: WILEY

摘要:

AbstractThe syntheses of the B‐norbenzomorphans, 1,5‐methano‐2,3,4,5‐tetrahydro‐1H‐2‐benzazepine (1a) and itsN‐methyl derivative (Ib) were accomplished. Phenylsuccinic anhydride (III) was cyclized to 3‐carboxy‐1‐indanone (IVa), which was converted by the Arndt‐Eistert method to the homologous methyl indanone‐3‐acetate (V). One experiment in the synthesis of V led to the by‐products 3‐carboxamido‐1‐indanone (IVd) and 3‐(N‐methylcarboxamido)‐1‐indanone (IVe), identified by physical and chemical means. Methyl 1‐aminoindan‐3‐acetate (VII) was prepared by catalytic reduction of methyl indanone‐3‐acetate oxime (VI). Hydrolysis of VII afforded 1‐aminoindan‐3‐acetic acid (VIII), which was cyclized with dicyclohexylcarbodiimide to 1,5‐methano‐2,3,4,5‐tetrahydro‐1H‐2‐benzazepin‐3‐one (IX). Reduction (lithium aluminum hydride) of IX gave amine Ia which was then methylated

ISSN:0022-152X    

DOI:10.1002/jhet.5570070404

出版商:Wiley‐Blackwell    

年代:1970

数据来源: WILEY

摘要:

Abstract2‐Methyl‐3‐(2‐pyridyl)quinoline (1) with a bromomethyl ketone or ethyl bromoacetate yields 6‐methyl‐12‐acylindolizino[1,2‐c]quinolinium bromides (5–9). The acyl derivatives can be deacylated in acid yielding 6‐methyl indolizino[1,2‐c]quinolinium salts (4). Benzoylation of4yields the 12‐benzoyl derivative (6).The deacylation product (4) has been synthesized from 2‐acetamidophenacyl bromide (10)

ISSN:0022-152X    

DOI:10.1002/jhet.5570070405

出版商:Wiley‐Blackwell    

年代:1970

数据来源: WILEY

摘要:

AbstractLes réactions de transalcoxylation des méthoxydiorganogermanes R2(H)GeOMe, avec des alcools éthyléniques et acétyléniques conduisent à des alcénoxy ou alcynoxygermanes du type. Ces dérivés à liaison germanium‐hydrogène subissent à la température ordinaire ou sous effet thermique, en présence ou non de catalyseurs platinés une cyclisation intramoléculaire prépondérante par addition du groupement Ge‐H sur l'insaturation carbone‐carbone. La structure des oxagermacycloalcanes de type furannique et pyrannique ainsi obtenus est confirmée par divers autres modes de synthèse. Les premiers oxagermacycloalcènes à double liaison carbone‐c

ISSN:0022-152X    

DOI:10.1002/jhet.5570070406

出版商:Wiley‐Blackwell    

年代:1970

数据来源: WILEY

摘要:

AbstractPolyphosphoric acid andN‐aryl‐N′‐benzoylethylenediamines in a type of Bischler‐Napieralski reaction afforded 1,2‐diaryl‐2‐imidazolines in good yields, rather than the 2,3‐dihydro‐1H‐[1,4]‐benzodiazepines. Blocking of the amino nitrogen by a methyl or ethyl group, to avoid imidazoline formation, gave starting material rather than the expected dihydrobenzodiazepine. Whenp‐tosyl was the blocking group, imidazoline was again the only product isolated. Analytical and spectroscopic data of several unreported 1,2‐diaryl

ISSN:0022-152X    

DOI:10.1002/jhet.5570070407

出版商:Wiley‐Blackwell    

年代:1970

数据来源: WILEY

摘要:

AbstractThe ribosylation of several silylated pyrrolo[2,3‐d]pyrimidines by the Wittenberg procedure has produced 1,3 and 7‐ribosylpyrrolo[2,3‐d]pyrimidine derivatives in high yield. Structure assignments have been made on the basis of the ultraviolet spectra of model compounds and further confirmed by chemical conversion to derivatives of established structure. A convenient ribosylation procedure utilizing silver oxide, a halosugar, and a silylated pyrrolo[2,3‐d]pyrimidine derivative in acetonitrile has been de

ISSN:0022-152X    

DOI:10.1002/jhet.5570070408

出版商:Wiley‐Blackwell    

年代:1970

数据来源: WILEY

摘要:

AbstractThe formation of 1‐substituted‐3‐hydroxy‐1H‐indazole and 1‐substituted‐benzimidazolin‐2‐one derivatives by thermal reaction ofN‐substituted‐N‐arylcarbam

ISSN:0022-152X    

DOI:10.1002/jhet.5570070409

出版商:Wiley‐Blackwell    

年代:1970

数据来源: WILEY

摘要:

AbstractSyntheses of 2,5‐disubstituted‐indazolones (Ixa–g) and 3‐hydroxy‐1‐substituted‐1H‐indazoles (XIVa,b) were achieved by diazotization of 2‐benzoylaniline (VIa–g) andN‐benzoylhydrazine (

ISSN:0022-152X    

DOI:10.1002/jhet.5570070410

出版商:Wiley‐Blackwell    

年代:1970

数据来源: WILEY