摘要:

AbstractStarting from 1–2 isopropylidene sn–glycerol, the synthesis of mono and diglycerides labelled with14C in the acyl moiety has been achieved.The acyl chloride method was found to be the best one for the esterification step.The various methods, hepe proposed with palmitic or lauric acid may be generalized for the obtention of other saturated glyceri

ISSN:0362-4803    

DOI:10.1002/jlcr.2580160202

出版商:John Wiley&Sons, Ltd.    

年代:1979

数据来源: WILEY

摘要:

Carbonatation of 3‐trifluoromethylthio phenylmagnesium bromide2with14CO2leads to (carboxyl‐14C) 3‐trifluoromethylthio benzoic acid3. Reduction of the latter with borane‐methyl sulfide complex (CH3)2S ‐ BH3in presence of trimethyl borate gives rise to 3‐tri‐fluoromethylthio benzyl alcohol4, which is oxidized by lead tetracetate in pyridine to give 3‐trifluoromethylthio benzaldehyde14CO5. The latter reacts with nitroethane to give 1‐(3′‐trifluoro methylthio phenyl)‐2‐nitropropene‐1‐14C6. This nitropropene is reduced by Fe‐HCl in presence of FeCl3into 1‐(3′‐trifluoromethyl‐thio phenyl)‐2‐propanone‐1‐14C7. Condensation of ethylamine with the ketone7followed by reduction in situ with sodium borohydride leads to 1‐(3′‐trifluoromethylthio phenyl)‐2‐ethylamino propane‐1‐14C8isolated as the hydrochloride. Specific activity: 47 mCi/mMol

ISSN:0362-4803    

DOI:10.1002/jlcr.2580160203

出版商:John Wiley&Sons, Ltd.    

年代:1979

数据来源: WILEY

摘要:

Abstract6β‐Iodomethyl‐19‐norcholest‐5(10)‐en‐3α‐ol (VI) was synthesized by the homoallylic rearrangement of 19‐iodocholest‐5‐en‐3α‐ol (V), which was obtained by the hydrolysis of 19‐iodocholest‐5‐en‐3α‐ol acetate derived from the displacement of cholest‐5‐ene‐3α,19‐diol 3‐acetate 19‐toluene‐p‐sulfonate with sodium iodide in isopropanol.The radioiodinated V and VI were prepared b

ISSN:0362-4803    

DOI:10.1002/jlcr.2580160204

出版商:John Wiley&Sons, Ltd.    

年代:1979

数据来源: WILEY

摘要:

Abstract[1‐14C]‐Trans‐9‐octadecenoic acid was obtained in 60 per cent overall yield and [9,10‐3H]‐trans‐9‐octadecenoic acid in 30 percent yield by stereomutation of the double bonds in the correspondingcis‐compounds with nitrous acid in toluene. The products were purified by silver nitrate chromatography and contained no detectable p

ISSN:0362-4803    

DOI:10.1002/jlcr.2580160205

出版商:John Wiley&Sons, Ltd.    

年代:1979

数据来源: WILEY

摘要:

AbstractThe preparation of the iodine‐125 labeled beta adrenergic antagonist, 1‐ (2′‐acetyl‐4′‐[ortho‐iodobenzoyl] ‐aminophenoxy)‐3‐isopropylamino‐propan‐2‐ol, suitable for biodistribution studies is described. Synthesis of the unlabeled precursor proceeds in a 44% yield and the iodine‐125 exchange results in 89% incorporation of label. The final product is radiochemically pure (98‐99%) with a s

ISSN:0362-4803    

DOI:10.1002/jlcr.2580160206

出版商:John Wiley&Sons, Ltd.    

年代:1979

数据来源: WILEY

摘要:

AbstractThe synthesis of the triply13C labeled molecule, diethyl 1‐[(13C)methyl]‐3‐Phenyl(1,3‐13C2)bicyclo[1.1.0]butane‐exo,exo‐2,4‐dicarboxylate is described. The unique feature of the synthesis is that in three instances we employed13CO2(from Ba13CO3) without using a high vacuum line. We found that excellent yields were obtained in two Grignard reagent carbonations and in a CO2reduction using a mechanical pump which produced a vacuum of 0.05 torr. The synthetic sequence involved carbonation of phenylmagnesium bromide to give (α‐13C)benzoic acid, reduction with LiAlH4, conversion to the corresponding benzyl chloride followed by preparation of the Grignard reagent and carbonation to produce phenyl (1,2,‐13C2)acetic acid. Reaction with13CH3Li provided 1‐Phenyl‐2‐(1,2,3‐13C3)‐propanone which, after conversion to its hydrazone and reaction with mercurous trifluoroacetate, yielded 1‐phenyl‐1‐(1,2,3‐13C3)propyne. Reaction twice with carboethoxycarbene (from ethyl diazoacetate) gave the des

ISSN:0362-4803    

DOI:10.1002/jlcr.2580160207

出版商:John Wiley&Sons, Ltd.    

年代:1979

数据来源: WILEY

摘要:

AbstractStarting with11CO2, [carboxyl‐11C]‐nicotinic acid amide was synthesized via 3‐pyridyl‐lithium in practically carrier‐free amounts within 60 minutes. Overall radiochemical yields between 20% and 30% were obtained. Identification and purification of the labelled product was carried out by high pressure liquid chromatography using water

ISSN:0362-4803    

DOI:10.1002/jlcr.2580160208

出版商:John Wiley&Sons, Ltd.    

年代:1979

数据来源: WILEY

摘要:

AbstractThe preparations of the pesticides 1,1a,2,2,3,3a,4,5,5,5a,5b,6‐dodecachlorooctahydro‐1,3,4‐metheno‐1H‐cyclobuta[cd]pentalene‐U‐C14(mirex‐U‐C14), 1,1a,3,3a,4,5,5,5a,5b,6‐decachlorooctahydro‐l,3,4‐metheno‐2H‐cyclobuta[cd]pentalen‐2‐one‐U‐C14(Kepone™‐U‐C14), ethyl 5‐(1,1a,3,3a,4,5,5,5a,5b,6‐decachlorooctahydro‐2‐hydroxy‐l,3,4‐metheno‐1H‐cyclobuta[cd]pentalen‐2‐Y1‐1,1a,2,3,3a,4,5,5a,5b,6‐C1410)‐ levulinate (kelevan‐C14), 1,4,5,6,7,8,8‐heptachloro‐3a,4,7,7a‐tetra‐hydro‐4,7‐methanoindene‐4,5,6,7,8‐C514(heptachlor‐4,5,6,7,8‐C514) and 1,4,5,6,7,8,8‐heptachloro‐2,3‐epoxy‐3a,4,7,7a‐tetrahydro‐4,7‐methanoindan‐4,5,6,7,8‐C514(heptachlor epoxide‐4,5,6,7,8‐C514) from hexachlorocyclopentadiene‐U‐C14are described. Specific activities were in the range of 1.8 to 3.2 mCi/mmol.Further, the synthesis of mirex‐C213and Kepone™‐C213from isopropyl formate‐C13is reported. The determination of the carbon‐13 enrichment of these compounds was accomplished by selected ion monitoring (SIM) of seven ions in the molecular clusters of mirex and Kepone™,

ISSN:0362-4803    

DOI:10.1002/jlcr.2580160209

出版商:John Wiley&Sons, Ltd.    

年代:1979

数据来源: WILEY

摘要:

AbstractCholesteryl esters of variously labelled fatty acids have been synthesized in high yield by 1,1′‐carbonyldiimidazole activation of the acyl group and reaction of the resulting acylimidazole derivative with cholesterol. The method has been used to synthesize cholesteryl esters on micro and semimicro scales. Syntheses of the following esters are reported: cholesteryl palmitate‐1‐14C, cholesteryl palmitate‐d31, cholesteryl palmitate‐2,2‐d2, cholesteryl palmitate‐d31, cholesteryl palmitate‐2,2‐d2, cholesteryl palmitate‐3,3,4,4,5,5,6,6,7,7,8,8,9,9,‐10,10,11,11,12,12,13,13,14,14,15,15,16,16,16‐d29, cholesteryl 5‐doxylpalmitate and c

ISSN:0362-4803    

DOI:10.1002/jlcr.2580160210

出版商:John Wiley&Sons, Ltd.    

年代:1979

数据来源: WILEY

摘要:

AbstractA three‐step synthesis of thymlne‐2,6‐13C2from urea‐13C, sodium cyanide‐13C, and α‐bromopropionic acid is described. The last reaction involves hydrogenation of α‐cyano‐13C‐propionylurea‐13C in aqueous acetic acid and produces thymine‐2,6‐13C2in 50–60% yield. The mechanism of

ISSN:0362-4803    

DOI:10.1002/jlcr.2580160211

出版商:John Wiley&Sons, Ltd.    

年代:1979

数据来源: WILEY