一种磷酸二甲啡烷中间体的制备方法

目的 探索一种适合工业化生产的磷酸二甲啡烷中间体的制备方法。方法 以5,6,7,8-四氢异喹啉为原料,采用一锅法,经甲基化、格氏反应、还原及拆分,得到磷酸二甲啡烷中间体(V),即d(4-甲基苯基)-2-甲基-1,2,3,4,5,6,7,8,-八氢异喹啉。 结果 制备的磷酸二甲啡烷中间体经¹H-NMR和MS谱等确证。总收率35.4%,纯度99.8%。 结论 该工艺收率提高,成本降低,操作简化,易于工业化生产。

Preparation of intermediate of dimemorfan phosphate

Objective To find out a method suitable for industrial manufacturing of intermediate of dimemorfan phosphate.MethodsWe took 5,6,7,8-tetrahydroisoquinoline as raw material,the intermediate of dimemorfan phosphate(V),that is, d(4-methylphenyl)-2-methyl-1,2,3,4,5,6,7,8,-octahydroisoquinoline,was prepared by methylation,Grignard reaction, reduction and chemical resolution with one-pot reaction.Results The intermediate of dimemorfan phosphate prepared was identified by ¹H-NMR and MS. The total yield was 35.4% and the purity was 99.8%. Conclusions The process is easy for synthesis, siutable for industrial manufacturing.