| Our study gives our own way to synthesize etrimfos. First, an intermediate a -Carbamoylacetimino-ethylester Hydrochloride is prepared wi th Cyanoacetamide as its raw material.then intermediate 6-ethoxy-2~ethyl-4-pyriraidinol is prepared with the first intermediate as its raw material. Finally, through the reaction of the second intermediate with 0, 0-d -imethylphosphorochloriclothionate, etrimfos is obtained.This paper studies mainly the synthesis of a -Carbamoyl-acetimino-Ethylester Hydrochloride and 6-ethoxy-2-ethyl-4-pyrimidinol, thus obtaining its better reaction conditions in our experiments. The structures of them are characterized by 1R, 'H-NMR and MS.The better reaction condions for a -Carbamoylacetimino-ethylester Hydrochloride are as follows: Reaction temperature is 15℃; The ratio of Cyanoacetamide to Ethylalcohol (molar ratio)is 1:1. 8;Dropping time of the solvent of Cyanoacetamide is 1 hour;The continual time of feeding MCI is also 1 hour;Continual reaction time is 2 hours.its yield is 77. 3%.The better reaction condions in which 6-ethoxy-2-ethyl-4-pyrimidinoJ is synthesized are as follows: The ratio of a -Carbamoylacetimino-ethylester Hydrochloride to Triethylamine is 1:3;Dropping time of the solvent of Propionyl chloride is 0. 5 hour, Dropping temperature of the solvent of Propionyl chloride is 20℃;Reaction temperature is 110℃.Its yieldis 29. 5%. |