摘要:

AbstractThe14C‐ring labeled carbinolamine N‐hydroxymethylpentamethyl‐melamine, a metabolite of the clinically useful anticancer agent hexamethylmelamine, was prepared in good yield from cyanuric chloride (ring, 2,4,6,‐14C). Amination of cyanuric chloride with dimethylamine gave 2‐chloro‐4,6‐bis(dimethylamino)‐1,3,5‐triazine‐2,4,6‐14C. Further amination with anhydrous methylamine gave pentamethylmelamine‐2,4,6‐14C. Condensation of pentamethylmethyl‐melamine with excess aqueous formaldehyde gave N‐hydroxymethylpentamethyl

ISSN:0362-4803    

DOI:10.1002/jlcr.2580211002

出版商:John Wiley&Sons, Ltd.    

年代:1984

数据来源: WILEY

摘要:

AbstractTwo synthetic routes lead to [14C] LF.1695. The first one starts with labelled triphenyl methyl phosphonium iodide. This Wittig reagent reacts with benzyl piperidinone to afford benzylmethylidene piperidine3. The reduction of3gives labelled pipecoline4which is condensed with an adduct affording an intermediate nitro compound5. LF.16956labelled at the methyl group is then obtained by catalytic reduction.The second route uses labelled chloro‐nitro benzoic acid as starting material. The treatment of the corresponding acid chloride by Friedel‐Crafts reaction gives the chloro‐nitro‐chloro‐benzophenone9in good yield. Condensation of9with pipecoline according to the method described above gives an intermediate nitro compound10which is reduced to afford LF.169511labelled at the carbo

ISSN:0362-4803    

DOI:10.1002/jlcr.2580211003

出版商:John Wiley&Sons, Ltd.    

年代:1984

数据来源: WILEY

摘要:

AbstractThe synthesis of [35S]‐labelled N‐sulpho‐2‐amino tricarballylate (SAT) and methods for its purification and analysis are described. In the first stage of the two‐step synthesis, chloro‐[35S]‐sulphonic acid is reacted with pyridine to yield pyridine‐[35S]‐sulphur trioxide. This agent is then utilized to sulphonate 2‐amino tricarballylic acid yielding the ultimate product [35S]‐SAT, which was required for ph

ISSN:0362-4803    

DOI:10.1002/jlcr.2580211004

出版商:John Wiley&Sons, Ltd.    

年代:1984

数据来源: WILEY

摘要:

AbstractThe synthesis and purification of carbon‐14 labeled capsaicin are describe

ISSN:0362-4803    

DOI:10.1002/jlcr.2580211005

出版商:John Wiley&Sons, Ltd.    

年代:1984

数据来源: WILEY

摘要:

AbstractA new apparatus was constructed to tritiate biological molecules using mass analysed tritium ion beams. The magnetic sector of this device was constructed of high field Sm‐Co permanent magnets. Mass analyzed ions of desired kinetic energy were impacted on an involatile solid and3H exchanged for H. The3H2+ions were found to be more reactive than3H2+ions. The sensitive peptide aldehyde leupeptin was utilized to test the efficacy of mass analyzed ion beam tritiation and leupeptin was not decomposed by this proces

ISSN:0362-4803    

DOI:10.1002/jlcr.2580211006

出版商:John Wiley&Sons, Ltd.    

年代:1984

数据来源: WILEY

摘要:

AbstractA method for the preparation of deuterium labelled unsymmetrical hydrazines was developed. This method was used to prepare l‐benzyl‐2‐methyl‐2H3‐hydrazine hydrobromide and l‐benzyl‐2H7‐2‐methylhydrazine hydrobromide, analogs of the cancer chemotheraputic agent procarbazine. These compounds were then used to prepare the corresponding labelled benzyl‐(ONN) and (NNO)‐azoxymethane isomers. A method was developed whereby the deuterium labelled azoxy isomers were separated by reversed phase

ISSN:0362-4803    

DOI:10.1002/jlcr.2580211007

出版商:John Wiley&Sons, Ltd.    

年代:1984

数据来源: WILEY

摘要:

Abstract4‐(2‐Chlorophenyl)‐1, 6‐dihydro‐1,3,9‐trimethylimidazo[1,2‐a]pyrazolo‐[4,3‐f] [1,4]diazepine‐9‐14C (CI‐918‐14C) was made starting with acetyl‐1‐14C chloride. An efficient synthesis of 1‐chloro‐2‐propanone‐2‐14C was developed as a precursor to 2‐methyl‐1,3‐dioxolane‐2‐14C‐2‐methanamine. The latter reacted with 4‐(2‐chlorophenyl)‐1,6‐dihydro‐1,3‐dimethylpyrazolo[3,4‐e] [1,4]diazepine‐7‐thione to yield 4‐(2‐chlorophenyl)‐1,6‐dihydro‐1, 3‐dimethyl‐N‐[(2‐methyl‐1,3‐dioxolan‐2‐yl‐2‐14C)methyl] pyrazolo[3,4‐e] [1,4]diazepin‐7‐amine. Hydrolysis and cyclization gave the title compound. The six‐step react

ISSN:0362-4803    

DOI:10.1002/jlcr.2580211008

出版商:John Wiley&Sons, Ltd.    

年代:1984

数据来源: WILEY

摘要:

AbstractWe describe the synthesis of tritiatedmeta‐aminolevamisole (MAL) of high specific radioactivity. Unlabelled MAL was iodinated with iodine monochloride in aqueous hydrochloric acid. The major reaction product, L[‐]2,3,5,6‐tetrahydro‐6‐(5‐amino‐2‐iodophenyl)imidazo [2,1‐b]thiazole, was catalytically dehalogenated with carrier‐free tritium gas in methanolic potassium hydroxide over 10% palladium‐carbon. After extraction and chromatography, a radioactive species ([3H]‐MAL) was identified with the same chromatographic mobility as unlabelled MAL, [3H]‐MAL possesses the same high biological activity in contracting nematode muscle as authentic unlabelled MAL, co‐chromatographs with unlabelled MAL in three different TLC systems and is about 90% radiochemically pure. By bioassay and competitive inhibition studies, the specific radioactivity of [3H]‐MAL appears greater than 15Ci/mmole and is probably close to 29Ci/mmole. [3H]‐MAL was shown to be useful for detecting a high affinity, saturable binding activity in extracts of the

ISSN:0362-4803    

DOI:10.1002/jlcr.2580211009

出版商:John Wiley&Sons, Ltd.    

年代:1984

数据来源: WILEY

摘要:

AbstractTwo complementary radiosynthetic routes to the potent PNMT inhibitor 7,8‐dichloro‐1,2,3,4‐tetrahydroisoquinoline‐1‐14C(1) from 2,3‐dichlorobenzaldehyde‐formyl‐14C(4) are described. In the Pomeranz‐Fritsch sequence isoquinoline6was prepared from Schiff's base5. Catalytic hydrogenation of6(H2/PtO2) furnished1in 28% radiochemical yield from4. In the aluminum chloride fusion sequence,4was converted via amino alcohol7to chloro amine8. Treatment of the latter with aluminum chloride/ammonium chloride (fusion, 190°C) yielded labeled1in 31% radioch

ISSN:0362-4803    

DOI:10.1002/jlcr.2580211010

出版商:John Wiley&Sons, Ltd.    

年代:1984

数据来源: WILEY

摘要:

Abstract1,8‐dihydroxy‐[10‐14C]9‐anthrone (anthralin) was synthesized in good yield starting from readily available 3‐methoxy‐2‐(2‐methoxybenzyl)‐benzoic acid (3).14C was introduced via carboxylation of the Grignard derived from 3‐bromo‐2(2‐methoxybenzyl) anisole. This, in turn, was obtained from (3) by a Curtius and Sand

ISSN:0362-4803    

DOI:10.1002/jlcr.2580211011

出版商:John Wiley&Sons, Ltd.    

年代:1984

数据来源: WILEY