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Synthesis of 3-hydroxy-N,N-dimethyl-cis-crotonamide dimethyl phosphate and its N-methyl analog labeled with 32P and 14C

✍ Scribed by W. B. Burton

Publisher
John Wiley and Sons
Year
1971
Tongue
French
Weight
715 KB
Volume
7
Category
Article
ISSN
0022-2135

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✦ Synopsis

Abstract

Two vinyl phosphates, 3‐hydroxy‐N,N‐dimethyl‐cis‐crotonamide dimethyl phosphate, and its N‐monomethyl analog, 3‐hydroxy‐N‐methyl‐cis‐crotonamide dimethyl phosphate, labeled with ^32^P and ^14^C in three positions, have been synthesized in milligram amounts. The radiosynthesis routes are reported and the effect of reduced scale preparation is discussed. As the compounds exist in geometric isomers, methods for their separation have been developed. The purity of the cis‐isomers was determined to be 98 to 99%. The yield of 3‐hydroxy‐N,N‐dimethyl‐cis‐crotonamide dimethyl phosphate labeled with ^32^P was 38%, with ^14^C‐O‐methyl 73% and with ^14^C‐N‐methyl 34%. The yield of 3‐hydroxy‐N‐methyl‐cis‐crotonamide dimethyl phosphate labeled with ^32^P was 38%, with ^14^C‐O‐methyl 73% and with ^14^C‐N‐methyl 80%.

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