摘要:

AbstractWe have synthesized14C‐ and2H‐labeled 1,3‐dihydro‐3,3‐dimethyl‐5‐(1,4,5,6‐tetrahydro‐6‐oxo‐3‐pyridazinyl)‐2H‐indol‐2‐one (LY195115), an extremely potent, orally‐effective cardiotonic with inotropic and vasodilator activities. The14C‐label was introduced in the antepenultimate step by reaction of a β‐chloroketone precursor with Na14CN; acid‐catalyzed hydrolysis and cyclization with hydrazine provided the tetrahydropyridazinone bearing the14C‐label in the oxo‐carbon. 1,3‐Dihydro‐3,3‐di(methyl‐d3)‐2H‐indol‐2‐one was prepared by exhaustive methylation of 1‐acetyl‐1,3‐dihydro‐2H‐indol‐2‐one with sodium hydride and iodomethane‐d3, followed by removal of the nitrogen protecti

ISSN:0362-4803    

DOI:10.1002/jlcr.2580230402

出版商:John Wiley&Sons, Ltd.    

年代:1986

数据来源: WILEY

摘要:

AbstractSynthetic procedures for the preparation of carbon‐14‐labeled sodium palmoxirate (TDGA), labeled either in the carboxyl position or in the tetradecyl hydrocarbon chain, are described. In addition, the synthesis of the coenzyme A ester of TDGA‐14Cwith a specific activity of 51 mCi/mmol is reported. The coenzyme A ester was prepared by formation of the acyl chloride with oxalyl chloride followed by reaction with coenzyme A (CoA) in a borate‐buffered tetrahydrofuran solution. Purification methods and analytical and stability data are reported for the co

ISSN:0362-4803    

DOI:10.1002/jlcr.2580230403

出版商:John Wiley&Sons, Ltd.    

年代:1986

数据来源: WILEY

摘要:

AbstractWe report the synthesis of tritiated 7‐dehydrocholesterol 5β,6β‐oxide in high specific activity. Oxidation of 7α‐bromo‐cholesterol 5β,6β‐oxide to the 3‐keto epoxide followed by borotritide reduction, in a special buffer‐organic solvent system to minimize undesired rearrangement, regenerated the 3β‐hydroxyl group. Base‐assisted elimination prod

ISSN:0362-4803    

DOI:10.1002/jlcr.2580230404

出版商:John Wiley&Sons, Ltd.    

年代:1986

数据来源: WILEY

摘要:

AbstractThe synthesis of [16‐3H]‐cembrene‐A from unlabelled cembrene‐A is achieved in four stepsviaselective hydroboration‐oxidation of the isopropenyl double bond, borotritide reduction of the 16‐aldehyde, ando‐nitroselenoxide elimination to regenerate the labelled olefin. This sequence is of general utility in labelling polyisoprenoid hydrocarbons for metabolic studies. Cembrene‐A is a putative intermediate in the conversion of geranylgeranyl pyrophosphate to the polycyclic trinervitane and kempane diterpenes of nasute t

ISSN:0362-4803    

DOI:10.1002/jlcr.2580230405

出版商:John Wiley&Sons, Ltd.    

年代:1986

数据来源: WILEY

摘要:

AbstractA method is described for the preparation and purification of 7‐[125I]‐Iodoclonazepam (5‐(o‐Chlorophenyl)‐2, 3‐Dihydro‐7‐[125I]‐Iodo‐1H‐1,4‐Benzodiazepin‐2‐one). The structure was confirmed by mass spectrometry using 7‐[127I]iodoclonazepam prepared by the same method. 7‐[125I]‐Iodoclonazepam binds well to a benzodiazepine antiserum. Although readily displaced by all the benzodiazepines commercially available in the UK, it is not displaced by structurally related nonbenzodiazepines except at very high concentrations. 7‐[125I]Iodoclonazepam should therefore be useful for the development of a screening radioim

ISSN:0362-4803    

DOI:10.1002/jlcr.2580230406

出版商:John Wiley&Sons, Ltd.    

年代:1986

数据来源: WILEY

摘要:

AbstractThe synthesis of [14C]Zolpidem, a new hypnotic agent having a non‐benzodiazepine structure, is described. This compound was synthesised in a 64% overall radio‐chemical yield from potassium[14C]cyanide and with a specific radioactivity of 56 mCi/mmol. It was used for pharmacokinetic and drug metabolism stud

ISSN:0362-4803    

DOI:10.1002/jlcr.2580230407

出版商:John Wiley&Sons, Ltd.    

年代:1986

数据来源: WILEY

摘要:

AbstractPolymeric [2H]‐formaldehyde, which is useful for the synthesis of a variety of labelled molecules, is prepared from bromoform in four steps. The isotopic purity of the final product depends on that of the [2H]‐bromoform made in the first step, and is measured after conversion of the [2H] formaldehyde to [2‐2H]‐5,5‐dimethyl‐

ISSN:0362-4803    

DOI:10.1002/jlcr.2580230408

出版商:John Wiley&Sons, Ltd.    

年代:1986

数据来源: WILEY

摘要:

AbstractSome vulcanizing accelerators, mercaptobenzothiazole derivatives labeled with carbon‐14 or sulfur‐35 were prepared. 2‐(Morpholinothio)benzothiazole labeled with carbon‐14 or sulfur‐35 of the sulfhydryl group at position 2 was synthesized by oxidative condensation with sodium hypochlorite from a mixture of morpholine and 2‐mercaptobenzothiazole‐2‐14C or 2‐mercaptobenzothiazole‐2‐35S. The same method was applicable to the synthesis of 2‐(morpholino‐U‐14C‐thio)‐benzothiazole using morpho

ISSN:0362-4803    

DOI:10.1002/jlcr.2580230409

出版商:John Wiley&Sons, Ltd.    

年代:1986

数据来源: WILEY

摘要:

AbstractPramiracetam (CI‐879;N‐[2[bis(1‐methylethyl)amino]ethyl]‐2‐oxo‐1‐pyrrolidineacetamide) was radiolabeled with tritium. Catalytic reduction of ethyl 2,5‐dihydro‐2‐oxo‐lH‐pyrrole‐1‐acetate in the presence of Pd/C gave ethyl 2‐oxo‐1‐[3,4‐3H]pyrrolidineacetate. Treatment of the tritiated ester withN,N‐bis(1‐methylethyl)‐1,2‐ethanediamine gave pramiracetam, which was subsequently

ISSN:0362-4803    

DOI:10.1002/jlcr.2580230410

出版商:John Wiley&Sons, Ltd.    

年代:1986

数据来源: WILEY

摘要:

Abstract4α‐(3H3)Methyl‐5α‐cholestan‐3β‐ol was regioselectively prepared from 5α‐cholest‐1‐en‐3‐oneviaalkylation with methyl iodide, hydrogenation, and LAH reduction. Details of this synthesis are given. The final and intermediate products were characterised b

ISSN:0362-4803    

DOI:10.1002/jlcr.2580230411

出版商:John Wiley&Sons, Ltd.    

年代:1986

数据来源: WILEY