SUMMARYA safe procedure for the conversion of barium carbonate-I4C to potassium cyanide-I4C on a 6-7 mmol scale in 90-98% yield was developed. Barium carbonate-14C was heated with excess potassium azide in a matrix of sand without added potassium metal, allowing safe, rapid and convenient recovery of the cyanide.
SUMMARYLithium borotritide reduction of a-ionylideneacetaldehyde (2) followed by manganese dioxide oxidation provided the tritiated aldehyde (2) which retained over 95% of the label. On treatment with the ylide derived from ethyl 4-chloro-3-methylcrotonate, ethyl a-retin~ate-ll-~H (14) was obtained which, after purification, was hydrolyzed to a-retin~ic-ll-~H acid hr (15). Conversion to the methyl ester (16) followed by lithium aluminum hydride reduction yielded a l l transa-retinal (17) which was isolated as the acetate derivative (18).
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