摘要
[目的]研究丙硫菌唑中间体1-氯-1-氯乙酰基环丙烷的合成工艺。[方法]以α-乙酰基-γ-丁内酯为原料,经氯化、水解一步合成3,5-二氯-2-戊酮,通过环合、氯化制得1-氯-1-氯乙酰基环丙烷。[结果]通过对单元反应的条件优化,确认了最佳合成工艺,4步反应总收率为76.7%,化合物结构经过~1H NMR和^(13)C NMR确证。[结论]该方法中α-乙酰基-γ-丁内酯的氯化产物不经分离,直接在酸液中水解;经碱液关环,在特殊催化剂甲醇少量存在下,氯化得到终产物。整个工艺路线流畅,反应收率高,具有较高工业应用价值。
[Aims] The aims were to study the synthesis of the intermediate for prothioconazole： 1-chloro-1-chloro- acetyl-cyclopropane. [Methods] With 2-acetylbutyrolactone as raw material, 3,5-dichloropentan-2-one was prepared by the process of chlorination and hydrolysis, and 1-ehloro-1-chloro-acetyl-cyclopropane was synthesized by the further cyclization and chlorination reaction. [Results] The optimized synthetic process was determined by optimization of reaction conditions for each step. The overall yield of four steps reaction was 76.7%, the product was determined by ^1H NMR and ^13C NMR. [Conclusions] 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 and in the ＇presence of special catalyst methanol. The whole process was smooth and the yield of the reaction was high with the high value for industrial application.
出处
《农药》
CAS
CSCD
北大核心
2018年第3期162-164,共3页
Agrochemicals
作者简介
王涛（1981-），男，河南扶沟人，讲师、注册安全工程师、化学检验技师，硕士，主要从事制药工程、应用化工和安全生产等方面教学研究工作。E—mail：94381286@qq．com。
