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目的改进硝酸依柏康唑的合成方法。方法以3,5-二氯溴苄为起始原料经Wittig反应、氢化、水解、环合4步反应得到关键中间体2,4-二氯-10,11-二氢-5H-二苯并[a,d]环庚烯-5-酮,该中间体经还原、氯代、氮烃化、成盐4步反应合成硝酸依柏康唑。结果与结论目标化合物的结构经质谱、核磁共振氢谱确证。与原工艺路线相比,改进后的路线反应步骤短、操作简单、条件温和,易于工业化生产,总收率为26%(以3,5-二氯溴苄计)。
Objective To improve the synthesis of ebicloconazole nitrate. Methods 3,5-Dichlorobenzyl bromide was used as the starting material to obtain the key intermediate of 2,4-dichloro-10,11-dihydro-5H-dibenzofuran by Wittig reaction, hydrogenation, hydrolysis and cyclization. [a, d] cyclohepten-5-one. The intermediate was reduced, chlorinated, and alkylated with nitrogen to form a salt. Results and Conclusions The structure of the target compound was confirmed by MS and 1H-NMR. Compared with the original process route, the improved routes have short reaction steps, simple operation, mild conditions and easy industrial production with a total yield of 26% (based on 3,5-dichlorobenzyl bromide).