摘要:

Abstract1‐(3,4‐Dirmethoxybenzyl)‐6, 7‐dimethoxyisoquinoline (papaverine) labeled with14C in either the benzyl or 4‐carbon position and 1‐(3,4‐dimethoxyphenyl) 6,7‐dimethoxyisoquinoline (quinopavine) labeled with14C at the 1,4 or 4‐methoxyphenyl position were synthesized. The 3,4‐dimethoxybenzoic acid‐carboxyl‐14C.(I) was, employed as the precursor in the synthesis of, all the above compounds except the 4‐methoxyphenyl labeled where 3‐methoxy‐4‐14C‐methoxybenzoic acid was employed (XII). The reduction of 3,4‐dimethoxybenzoylchloride14C (VII) led to the formation of 3,4‐dimethoxybenzaldehyde‐carbonyl14‐C (VIII) from which 2‐(3,4‐dimethoxyphenyl)‐2‐methoxyethylamine‐2‐14C (XI) was obtained through reduction of the corresponding14C‐labeled substituted nitrostyrene (IX). 3,4‐Dimethoxybenzoic acid‐carboxyl‐14C (I) was employed in the synthesis of (3,4‐dimethoxyphenyl)‐acetonitrile‐2‐14C (IV) from which a) 2‐(3,4‐dimethoxyphenyl)‐ethylamine‐2‐14C (VI) was obtained on reduction and b) (3,4‐dimethoxyphenyl)‐acetic acid‐2‐14C (V) on alkaline hydrolysis. On heating together at 200°C the corresponding acids and amines in the absence as well as in the presence of decaline (solvent), or by a Schotten‐Bawmann reaction, the corresponding amines were obtained and them cyclized in the presence of phosphorus oxychloride. The 3, 4‐dihydro‐products were dehydrogenated in the presence of palladium‐pumice which acted as a catalyst. The cyclization of N‐(3,4‐dimethoxyphenyl‐2‐methoxyethyl‐2‐14C) 3,4‐dimethoxyphenyl‐acetamide (XVI) gave straightway t

ISSN:0022-2135    

DOI:10.1002/jlcr.2590100302

出版商:John Wiley&Sons, Ltd.    

年代:1974

数据来源: WILEY

摘要:

AbstractThe synthesis of3H and14C labeledd‐2‐ethyl‐2‐phenyl‐4‐(2‐piperidyl)‐1, 3‐dioxolane hydrochloride (Va and Vb respectively) is described. The optically pure α(‐)‐2‐(2‐piperidyl)ethane‐1,2‐diol hydrochloride (II), obtained by hydrolyzing α (+)‐2,2‐diphenyl‐4‐(2‐piperidyl)‐1,3‐dioxolane hydrochloride(1)(I), is used as the starting material to minimize the n

ISSN:0022-2135    

DOI:10.1002/jlcr.2590100303

出版商:John Wiley&Sons, Ltd.    

年代:1974

数据来源: WILEY

摘要:

AbstractDiazepam‐14C and demethyldiazepam‐14C are synthesized from glycine‐1‐14C. Addition of diketene to diazepam‐14C leads to ketazolam‐14C. The reaction conditions for the formation of ketazolam from diazepam is studied using high‐pressure liquid chromatography in conjunction with radioactivity d

ISSN:0022-2135    

DOI:10.1002/jlcr.2590100304

出版商:John Wiley&Sons, Ltd.    

年代:1974

数据来源: WILEY

摘要:

AbstractA modification of the Sandmeyer reaction which requires only a moderate excess of cyanide‐14C was utilized for the preparation of 4‐chloro‐2‐fluorobenzonitrile‐7‐14C (3). After hydrolysis, the resulting acid (4) was converted to carboxy labelled furosemide (6) by existing methods. This procedure is potentially useful for insertion of14C in compounds that fail to undergo conventional carbonatio

ISSN:0022-2135    

DOI:10.1002/jlcr.2590100305

出版商:John Wiley&Sons, Ltd.    

年代:1974

数据来源: WILEY

摘要:

AbstractThe preparation of 1‐[ (3′‐14C)‐Allyl]‐3,4‐methylene dioxy‐,1‐[(3′‐14C)‐allyl]‐3‐methoxy‐4,5‐methylene dioxy‐, and 1‐[(3′‐14C)‐allyl]‐3,4,5‐trimethaoxy benzenes is described. The14C‐label was introduced into the 3′‐carbon

ISSN:0022-2135    

DOI:10.1002/jlcr.2590100306

出版商:John Wiley&Sons, Ltd.    

年代:1974

数据来源: WILEY

摘要:

AbstractIt it shown that the photo‐oxidation of aromatic molecules containing an active methylene group can be used to introduce isotopic oxygen. Photo‐oxidation of xanthene results in the formation of xanthone with the oxygen label appearing in the product at the carbonyl group. In this way, 100% enrichment can be realized. A brief discussion of other systems to which this method may be extended is also gi

ISSN:0022-2135    

DOI:10.1002/jlcr.2590100307

出版商:John Wiley&Sons, Ltd.    

年代:1974

数据来源: WILEY

摘要:

AbstractA method is described by which18O‐DMF can be prepared conveniently and in very high yields (∼ 90%) by reacting at room temperature an equimolar quantity of benzoyl chloride, DMF and18O‐labelled

ISSN:0022-2135    

DOI:10.1002/jlcr.2590100308

出版商:John Wiley&Sons, Ltd.    

年代:1974

数据来源: WILEY

摘要:

AbstractThe preparation of ethyl 6‐ethyl‐4‐hydroxy[3‐14C] cinnol‐3‐ul carboxylate (ICI 75,186) from diethyl[2‐14C]malonate in five stages is described, together with the purification procedures involved. The overall radiochemical yield, at a specific activity of 3.3 μ

ISSN:0022-2135    

DOI:10.1002/jlcr.2590100309

出版商:John Wiley&Sons, Ltd.    

年代:1974

数据来源: WILEY

摘要:

AbstractSynthesis of 6‐/N,N‐1′, 6′‐hexyleneformamidine‐14C/penicillanic acid /VII/ was carried out. N‐formyl‐14C‐hexamethyleneimine /II/ was obtained from formic‐14C acid and hexamethyleneimine /I/. The product was chlorinated with oxalyl chloride. The obtained N,N‐1, 6‐hexylenechloroformimino‐14C chloride /III/ was condensed with trimethylsilyl ester of N‐trimethylsilyl‐6‐amino penicillanic acid /V/. The final product /VII/ was separated with

ISSN:0022-2135    

DOI:10.1002/jlcr.2590100310

出版商:John Wiley&Sons, Ltd.    

年代:1974

数据来源: WILEY

摘要:

AbstractFluothane (1, 1, 1‐trifluoro‐2‐chloro‐2‐bromoethane) is a well known anesthetic, and its labeled compound has been much required for the biological investigation. The method was studied to prepare fluochane‐82Br by means of recoil labeling. More than 20 organic species labeled with bromine‐82 evolved in neutron‐irradiated fluothane. From such the complicated system, however, fluothane‐82Br was purely obtained by the gas chromatographic separation. Under the optimum conditions, the radiochemical yield of fluothane‐82Br contributed to 38%.When 200 μl of the target material was irradiated with neutrons to the total neutron dose (nvt) of 3.4 × 1016n/cm2, the radioactivity of82Br‐labeled fluothane isolated almost quantitat

ISSN:0022-2135    

DOI:10.1002/jlcr.2590100311

出版商:John Wiley&Sons, Ltd.    

年代:1974

数据来源: WILEY