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盐酸达泊西汀的合成及工艺优化
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| 篇名： | 盐酸达泊西汀的合成及工艺优化 |
| TITLE： | Synthesis and Technology Optimization of Dapoxetine Hydrochloride |
| 摘要： | 目的：优化盐酸达泊西汀的合成工艺。方法：采用手性合成的方法，以3-氯苯丙酮为原料，采用（1S，2R）（--）-1-氨基-2-茚醇为催化剂、硼烷-N，N-二乙基苯胺为还原剂进行不对称还原，然后依次经过与α-萘酚醚化、磺酸酯化、二甲胺取代、HCl成盐反应得到最终产物。通过核磁共振和质谱技术对合成产物进行表征。对中间体Ⅰ、中间体Ⅱ、中间体Ⅲ和最终产物的合成反应进行工艺优化。结果：表征结果显示最终产物为盐酸达泊西汀，纯度为99.8％，收率为58.9％。与传统的拆分工艺比较，本工艺采用手性合成的方法不需要拆分，收率明显高于文献报道的拆分工艺收率（31.9％）。优化后的工艺减少了杂质的产生，提高了产品质量。结论：本合成工艺反应条件较温和、合成路线较短、收率较高。 |
| ABSTRACT： | OBJECTIVE：To optimize the synthesis process of dapoxetine hydrochloride. METHODS ：By chiral synthesis ， asymmetric reduction was carried out by using 3-chlorophenylacetone as raw material ，（1S，2R）-（-）-1-amino-2-indanol as catalyst，and borane- N，N-diethylaniline （DEANB） as reducing agent. Then ，it was reacted with α-naphthol etherification， sulfonation，dimethylamine substitution ，and HCl salt formation reaction to obtain the final products. The products were characterized by NMR and MS. The synthesis reaction of intermediate Ⅰ，intermediate Ⅱ，intermediate Ⅲ and the final product were optimized. RESULTS ：The final product was dapoxetine hydrochloride with purity of 99.8％ and yield of 58.9％. Compared with traditional splitting technology ，the chiral synthesis technology of this study did not need splitting ，and the yield of the technology was significantly higher than that of splitting technology reported in literature （31.9％）. The optimized technology reduced the generation of impurities and improved the product quality. CONCLUSIONS ：The improved technology has milder reaction conditions ，shorter synthesis route and higher yield. |
| 期刊： | 2020年第31卷第07期 |
| 作者： | 付丙月，张宁，张宗磊，段崇刚 |
| AUTHORS： | FU Bingyue ，ZHANG Ning，ZHANG Zonglei ，DUAN Chonggang |
| 关键字： | 盐酸达泊西汀；手性合成；不对称还原；工艺优化 |
| KEYWORDS： | Dapoxetine hydrochloride ；Chiral synthesis ；Asymmetric reduction ；Technology optimization |
| 阅读数： | 1512 次 |
| 本月下载数： | 29 次 |
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