盐酸苯海索的合成工艺改进

Process improvement on the synthesis of trihexyphenidyl hydrochloride

目的通过优化工艺,提高盐酸苯海索生产安全性和产品收率。方法用金属镁和氯代环己烷制备格氏试剂,再与中间体盐酸哌啶苯丙酮发生加成反应,最后加盐酸水解得到盐酸苯海索,本研究采用单一因素法深入讨论了原料配比、溶剂用量、格氏反应温度、格氏反应时间对产物收率的影响。结果经过工艺参数优化,盐酸苯海索的收率由之前的30%左右提高到了50%以上。结论原工艺经过优化后,生产较为安全,减少了原料的损失,提高了粗品的收率,为工业化生产奠定了基础。

ObjectiveTo improve the production safety and increase the product yield of benzhexol hydrochloride by process optimization.Methods Firstly, preparing grignard reagent with magnesium and chlorocyclohexane; then adding piperidylpropiophenone hydrochloride to carry out the additive reaction; finally, adding hydrochloric acid, by its hydrolyzing, we get the benzhexol hydrochloride. In this paper, the effects of raw material ratio, solvent dosage, grignard reaction temperature and grignard reaction time on the product yield were in-depth discussed with the single-factor method.Results By process optimization, the product yield of benzhexol hydrochloride increased from 30% to more than 50%. Conclusion The process optimization improves the production safety, reduces the loss of raw materials, and raises the raw product yield, which therefore lays the foundation for industrial production.