Lan Zhi-li
2011
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Journal
Agrochemicals Research & Application
Abstract
5-(1-methylthio)ethyl-2-(trifluoromethyl)pyridine(3)was synthesized from 1-(3-methylthiobut-1-phenyl)pyrrolidine(1)and 4-ethoxy-1,1,1-trifluoro-but-3-en-2-one(2)in the protection of nitrogen and presence of ammonium formate. The yield of the reaction was about 63.5% with the purity of 98.6%. The effect of the reaction conditions on reaction yield was investigated,and the optimal conditions were as follows:the material ratio of n(1-(3-methylthiobut-1-phenyl)pyrrolidine)∶n(4-ethoxy-1,1,1-trifluoro-but-3-en-2-one)∶ n(ammonium bicarbonate)=0.9∶1.0∶2.2,reaction solvent was acetonitrile,the solvent amount was 250 mL/mol,calefactive reaction temperature was 75 ℃,total reaction time was 4.5 hours.