[Objective] The paper was to study the synthesis technology of the intermediate for prothioconazole： 1-chloro-1-chloroacetyl-cyclopropane. [Method] With 2-acetylbutyrolactone as the raw material, 3,5-dichloro-2-penta...[Objective] The paper was to study the synthesis technology of the intermediate for prothioconazole： 1-chloro-1-chloroacetyl-cyclopropane. [Method] With 2-acetylbutyrolactone as the raw material, 3,5-dichloro-2-pentanone was synthesized by chlorination and hydrolysis, and1-chloro-1-chloroacetyl-cyclopropane was synthesized by further cyclization and chlorination. [Result] The optimized synthetic process was determined by optimizing reaction conditions of each step. The overall yield of four-step reaction was 76.7%, and the product was verified by1 H NMR and13 C NMR. [Conclusion] The chlorinated product of 2-acetylbutyrolactone was directly hydrolyzed in acid solution without separation, and the final product was obtained by chlorination of cyclization product in the presence of special catalyst methanol. The whole process was smooth and the yield of the reaction was high, with high value for industrial application.展开更多
基金Supported by National Natural Science Foundation of China(30870109)
文摘[Objective] The paper was to study the synthesis technology of the intermediate for prothioconazole： 1-chloro-1-chloroacetyl-cyclopropane. [Method] With 2-acetylbutyrolactone as the raw material, 3,5-dichloro-2-pentanone was synthesized by chlorination and hydrolysis, and1-chloro-1-chloroacetyl-cyclopropane was synthesized by further cyclization and chlorination. [Result] The optimized synthetic process was determined by optimizing reaction conditions of each step. The overall yield of four-step reaction was 76.7%, and the product was verified by1 H NMR and13 C NMR. [Conclusion] The chlorinated product of 2-acetylbutyrolactone was directly hydrolyzed in acid solution without separation, and the final product was obtained by chlorination of cyclization product in the presence of special catalyst methanol. The whole process was smooth and the yield of the reaction was high, with high value for industrial application.
