| 李强国,戚太林.一种磷酸二甲啡烷中间体的制备方法[J].安徽医药,2016,20(1):41-42. |
| 一种磷酸二甲啡烷中间体的制备方法 |
| Preparation of intermediate of dimemorfan phosphate |
| 投稿时间：2015-09-12 |
| DOI： |
| 中文关键词: 磷酸二甲啡烷 中间体 一锅法 工业化生产 |
| 英文关键词: dimemorfan phosphate intermediate one-pot reaction industrial manufacturing |
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| 中文摘要: |
| 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。 |
| 英文摘要: |
| 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. |
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