摘要:

not available

ISSN:0008-4042    

DOI:10.1139/v68-496

出版商:NRC Research Press    

年代:1968

数据来源: NRC

摘要:

The chemistry of 1,2,3,7,8,12b-hexahydro-, 1,7,8,12b-tetrahydro-, and 7,8-dihydrobenzo[1,2]cyclohepta[3,4,5-d,e]isoquinolines has been investigated, leading to the synthesis of a wide variety of derivatives bearing substituents in the 2- and 3-position. Also, the reactions of 1,7,8,12b-tetrahydrobenzo[1,2]cyclohepta[3,4,5-d,e]isoquinoline with 1-buten-3-one, methyl mercaptoacetate, and 3-mercaptopropionic acid have yielded representatives of three novel pentacyclic systems; benzo[4,5]cyclohepta[1,2,3-g,h]-benzo[a]quinolizine, benzo[1,2]cyclohepta[3,4,5-d,e]thiazolo[2,3-a]isoquinoline, and benzo[1,2]cyclohepta[3,4,5-d,e]-1,3-thiazino[2,3-a]isoquinoline. The central nervous system and cardiovascular pharmacology of the compounds have been investigated and the results are presented.

ISSN:0008-4042    

DOI:10.1139/v68-497

出版商:NRC Research Press    

年代:1968

数据来源: NRC

摘要:

The nuclear magnetic resonance (n.m.r.) spectra ofN,2,6-trichloro-p-benzoquinone imine (1) and the anisotropy effect of the chloroimino group are investigated. A comparison of the n.m.r. spectra of1with those of oximes with a similar structure shows that the extent of the anisotropy effect is the same for both the chloroimino and the hydroxyimino group. This is also confirmed by comparison ofN-chlorocyclohexanimine with cyclohexanone oxime. A downfield shift of the C—H proton signal in solvents acting as a base is observed, which is interpreted in terms of abase hydrogen bond. The extent of the shift is different betweensynandantisides and this gives the definite assignment for these two types of proton signals. Namely, the high-field signal, the extent of the downfield shift being larger, is assigned toantiprotons, and the low-field one tosynprotons. This assignment is extended to oximes owing to the equality of the anisotropy effects of the hydroxyimino and the chloroimino group. The formation of thebase hydrogen bond is confirmed by the infrared (i.r.) spectra, and the correlation between the extents of n.m.r. downfield shift and i.r. low wave number shift is discussed. Furthermore it is found that the behavior of benzene molecule as solvent is different between the chloroimino and the hydroxyimino compounds.

ISSN:0008-4042    

DOI:10.1139/v68-498

出版商:NRC Research Press    

年代:1968

数据来源: NRC

摘要:

Dehydrochlorination of 3,4,6-tri-O-acetyl-2-chloro-2-deoxy-α-D-glucopyranosyl chloride with diethyl-amine yielded 3,4,6-tri-O-acetyl-2-chloro-D-glucal. The latter was further chlorinated to 3,4,6-tri-O-acetyl-2-deoxy-2,2-dichloro-α-D-ararbino-hexopyranosyl chloride, which on deacetylation provided the first example of a stable, free glycopyranosyl chloride.A 3,4,6-tri-O-acetyl-2-chloro-2-deoxymannopyranosyl chloride, also isolated in this work, was characterized by properties which correspond closely to the recently reassigned β anomer.

ISSN:0008-4042    

DOI:10.1139/v68-499

出版商:NRC Research Press    

年代:1968

数据来源: NRC

摘要:

DL-threo- andDL-erythro-β-Hydroxyisoleucine were prepared fromcis- andtrans-3-methylpent-2-enoic acids, respectively. The configuration of theerythroisomer was established from its synthesis by two independent routes. The diastereoisomers, and those of other β-hydroxy amino acids, can be distinguished by examination of their proton magnetic resonance spectra.

ISSN:0008-4042    

DOI:10.1139/v68-500

出版商:NRC Research Press    

年代:1968

数据来源: NRC

摘要:

Several α-hydrazino carboxylic acids and theirm-nitrobenzal hydrazones have been prepared and characterized. The latter and two of the former have not been previously reported. The α-hydrazino acids were found to react with ninhydrin to yield Ruhemann's purple, but in much lower yield than the corresponding amino acids. However, hydrazine itself yields a different colored product. Various aspects of the reaction between ninhydrin and the α-hydrazino acids were investigated and a mechanism for the formation of Ruhemann's purple is suggested.

ISSN:0008-4042    

DOI:10.1139/v68-501

出版商:NRC Research Press    

年代:1968

数据来源: NRC

摘要:

not available

ISSN:0008-4042    

DOI:10.1139/v68-502

出版商:NRC Research Press    

年代:1968

数据来源: NRC

摘要:

Amperometric titration with methylmercuric iodide was found to be unsatisfactory for the quantitative determination of —SH and —SS— values in several soluble proteins. It is concluded that the "high reactivity" of the mercurial has previously been overemphasized. Consistent values can, however, be obtained by permitting protein samples to react with an excess of the mercurial, for about 100 h, followed by the polarographic estimation of the remaining reagent. Contrary to general belief, this procedure was found to be more precise than amperometric titration, and, if appropriate precautions are taken, it is applicable to considerably smaller amounts (<0.5 μmole —SH or —SS—) of either soluble or insoluble protein. The necessary experimental procedure is described and results are reported for several proteins. For the compounds studied, methylmercuric iodide did not react at non-sulfhydryl sites, and did not additionally bind to the mercaptides formed; there was no indication of disulfide bond cleavage, despite the long reaction times used.

ISSN:0008-4042    

DOI:10.1139/v68-503

出版商:NRC Research Press    

年代:1968

数据来源: NRC

摘要:

Lithium naphthalene reacts easily with terminal acetylenic hydrocarbons, such as acetylene, methyl-acetylene, or phenylacetylene, to give the corresponding lithium compounds quantitatively. The reaction of these lithium compounds with α,β-unsaturated ketones gives the corresponding acetylenic carbinols in a good yield under mild conditions.

ISSN:0008-4042    

DOI:10.1139/v68-504

出版商:NRC Research Press    

年代:1968

数据来源: NRC

摘要:

The interaction between aromatic and aliphatic nitro compounds in basic media has been investigated. Evidence based mainly on nuclear magnetic resonance spectroscopy suggests that the brightly colored species formed are sigma complexes. The generality of the reaction is investigated and its relation to the Janovsky reaction discussed.

ISSN:0008-4042    

DOI:10.1139/v68-505

出版商:NRC Research Press    

年代:1968

数据来源: NRC