摘要:

AbstractA large body of organic compounds containing carbon‐hydrogen bonds have very feeble acidic properties. In order that these compounds be made to ionise it is necessary to employ highly basic media. Recent developments now result in the use of several such systems, some of which can serve as a convenient source of labelling. The possibilities of the method are outlined together with the limitations, and a number of specific examples illustrating how compounds can be labelled are give

ISSN:0022-2135    

DOI:10.1002/jlcr.2590040302

出版商:John Wiley&Sons, Ltd.    

年代:1968

数据来源: WILEY

摘要:

AbstractA synthesis of meta‐terphenyl‐2,4,6,2′,5′,2″,4″,6″‐D8has been carried out. From iodobenzene‐2,4,6‐D3and 2,6‐dibromo‐1,4‐dinitrobenzene, the compound 2′,5′‐dinitro‐meta‐terphenyl‐2,4,6,2″,4″,6″‐D6is formed (Ullmann reaction). By reduction of the nitrogroups and subsequent reductive diazotization, two deuterium atoms are introduced into the centre ring at positions 2′ and 5′. The labelled meta‐terphenyl has been obtained in 15 % yield, based on labelled iodobenzene. Deuterium substitution is ≥ 98% at positions 2,4,6

ISSN:0022-2135    

DOI:10.1002/jlcr.2590040303

出版商:John Wiley&Sons, Ltd.    

年代:1968

数据来源: WILEY

摘要:

AbstractDeuterium chemistry is still quite costly, mainly because of the high prices of deuterated compounds needed for syntheses. Furthermore, the risk of diluting isotopically the compounds prepared is considerable. These disadvantages can be alleviated, if i) the deuterium of the D‐donator is exchanged efficiently, ii) highly deuterated solvents and reactants can is be prepared conveniently on a laboratory scale, and iii) compounds, which have been isotopically diluted can be reconcentrated conveniently. Fulfillments of these requirements allows for research in deuterium chemistry on a close to pilot plant scale at tolerable costs.With this aim in mind, basic principles of batch deuterations on pilot plant scale with low grade heavy water discussed. By up‐grading D2O wastes, close to 98 % of the deuterium employed for reaction can be incorporated into the substr

ISSN:0022-2135    

DOI:10.1002/jlcr.2590040304

出版商:John Wiley&Sons, Ltd.    

年代:1968

数据来源: WILEY

摘要:

AbstractA method for the biosynthesis of15N‐labelled S‐adenosylmethionine from15NH4+and L‐methionine by yeast is reported. Culture conditions suitable for economy in the utilization of the isotope were developed, and the use of γ‐irradiated yeast (1 Mrad) for this purpose was explored. The irradiated yeast proved as effective as non‐irradiated yeast, but it did not offer any advantage.15N‐Adenine was obtained from S‐adenosylmethionine by hydrolysis; its isolation by ion exchange chromatograph

ISSN:0022-2135    

DOI:10.1002/jlcr.2590040305

出版商:John Wiley&Sons, Ltd.    

年代:1968

数据来源: WILEY

摘要:

AbstractL'acide benzoïque carboxyle 14C (5 mM) est réduit par LiAlH4en alcool benzylique14C‐7. L'oxydation de ce dernier par le tétracétate de plomb dans la pyridine donne le benzaldéhyde14CO lequel, sans être isolé, est condensé avec l'acide malonique. L'acide cinnamique14C‐3 obtenu avec un rendement global de 86%, purijié par sublimation est homogtke dans trois solvants de chromatographie sur papier. Activité spécifi

ISSN:0022-2135    

DOI:10.1002/jlcr.2590040306

出版商:John Wiley&Sons, Ltd.    

年代:1968

数据来源: WILEY

摘要:

AbstractDiethyl acetamidomalonate‐2‐14C was alkylated by l‐chloromethylpyrazole and the reaction intermediate hydrolyzed to give DL‐3‐(1′‐pyrazolyl)‐alanine‐2‐14C. By the same method, but using 3‐chloromethylpyrazole instead of the 1‐isomer, DL‐3‐(3′‐pyrazolyl)‐alanine‐2‐14C was prepared. Condensation of furfural with hydantoin‐5‐14C gave 5‐(2′‐furylidene)‐hydantoin‐5‐14C, which was subsequently reduced to 5‐(2′‐furyl)‐hydantoin‐5‐14C and this compound was hydrolyzed to DL‐3‐(2′‐furyl)‐alanine‐2‐14C. Methods f

ISSN:0022-2135    

DOI:10.1002/jlcr.2590040307

出版商:John Wiley&Sons, Ltd.    

年代:1968

数据来源: WILEY

摘要:

Allylacetic acid 1‐14C prepared by carbonation of 3‐butenyl‐magnesium bromide is oxidized into succinic acid 1‐14C by periodic acid and a catalytic amount of K MnO4. After purification by chromatography on a column of Dowex 1 × 10 Cl−, succinic acid 1‐14C is secured with an over all yield of 66 % based on Ba14CO3specific activity 37.4 mCi /mM. This method is more convenient than those of the literature because it avoids the preparation of K14CN and affords a better yield.L'acide allylacétique (carboxyl14C) obtenu par carbonatation du bromure de butène‐3 ylmagnésium est oxydé en acide succinique (14C‐1) par l'acide periodique en présence de quantités catalytiques de permanganate de potassium. Après purification par chromatographie sur résine échangeuse Dowex 1 × 10 Cl−, l'acide succinique (14C‐1) est obtenu avec un rendement global de 66 % calculé sur14CO3Ba; activité spécifique 37,4 mCi/mM. Les avantages de cette méthode sur celles de la littérature sont d'éviter la préparaation du cyanure de potassium

ISSN:0022-2135    

DOI:10.1002/jlcr.2590040308

出版商:John Wiley&Sons, Ltd.    

年代:1968

数据来源: WILEY

摘要:

DL Arginine (14C‐1) is prepared by a Strecker reaction with γ‐guanidobutyraldehyde and K14CN. Radioactive and chemical yields are 60 % based on K14CN.La DL‐Arginine (14C‐1) a été obtenue par réaction de Strecker à partir de l'aldéhyde γ‐guanido butyrique et du cyanure de potassium (14C) avec des rendements chimiques et radioactifs de l'ordre de 60 % par

ISSN:0022-2135    

DOI:10.1002/jlcr.2590040309

出版商:John Wiley&Sons, Ltd.    

年代:1968

数据来源: WILEY

摘要:

Carbonation ofp‐bromophenylmagnesium chlorure with14CO2leads to p‐chlorobenzoic acid carboxyl14C (1) with a 97 % yield. The latter, treated in a sealed tube by concentrated ammonia in presence of sodium iodide and cuprous chloride at 140° C provides p‐aminobenzoic acid caboxyl14C (2) with a 67 % yield. The synthesis proceeds by diazotation in fluoboric acid in order to obtain p‐carboxy‐14C benzenediazonium fluoborate (3). This salt, treated in acetone, water solution, by a mixture of mercuric chloride and stannous chloride leads to the final compound (4). It is purified by extraction in D. M. F. and precipitation by water addition. Overall yield is 51 % based on (2) or 30–35 % based on Ba14CO3. Specific activity: 10 mCi/mM. The radiochemical purity has been checked by paper radiochromatography.La carbonatation par14CO2du chlorure de p‐bromophénylmagnésium donne l'acide p‐chlorobenzoïque (carboxyle14C) (1) avec un rendement de 97 %. Ce dernier est ensuite traité en tube scellé par l'ammoniaque en présence d'iodure de sodium et de chlorure cuivreux à 140°C, ce qui fournit l'acide p‐aminobenzoïque (carboxyle14C) (2) avec un rendement de 67 %. La synthèse se poursuit par la diazotation dans l'acide fluoborique pour obtenir le fluoborate de p‐carboxy‐14C benzènediazonium (3); ce sel, traité en solution dans l'acétone aqueuse, par le mélange chlorure mercurique, chlorure stanneux conduit au produit final (4) qui est purifié par extraction dans le D. M. F. et précipitation par l'eau. Le rendement global est de 51 %; par rapport à (2), soit 30–35 % par rapport à14CO3Ba. Activité spécifique : 10mCi/mM. La pureté radiochimique a ét

ISSN:0022-2135    

DOI:10.1002/jlcr.2590040310

出版商:John Wiley&Sons, Ltd.    

年代:1968

数据来源: WILEY

摘要:

AbstractDie14C‐ und3H‐Markierung von 1‐Phenyl‐4‐amino‐5‐chlor‐6‐pyridazon im Phenylring wurde durch Umsetzung von Mucochlorsäure mit14C‐bzw.3H‐markiertem Phenylhydrazin‐hydrochlorid und Erhitzen des markierten Zwischenproduktes 1‐Phenyl‐4,5‐dichlor‐6‐pyridazon mit konzentriertem Ammoniak erzielt. Die Synthese mit14C‐markierter Mucochlorsäure als Ausgangs‐material ergab Markierung im Pyridazonring.14C‐ und3H‐markiertes Phenylhydrazin‐hydrochlorid wurde aus markiertem Anilin‐hydrochlorid synthetisiert und14C‐markierte Mucochlorsäure wurde aus Acetylen‐14C oder Formaldehyd‐14C mit14C‐mar

ISSN:0022-2135    

DOI:10.1002/jlcr.2590040311

出版商:John Wiley&Sons, Ltd.    

年代:1968

数据来源: WILEY