[關(guān)鍵詞]
[摘要]
目的 對咪達那新的合成工藝進行研究。方法 以二苯乙腈為起始原料,與1,2-二溴乙烷經(jīng)相轉(zhuǎn)移反應生成4-溴-2,2-二苯基丁腈(1),化合物1在三乙胺存在下,于N,N-二甲基甲酰胺–二甲基亞砜中與2-甲基咪唑反應,生成4-(2-甲基-1H-咪唑-1-基)-2,2-二苯基丁腈(2),化合物2在70%硫酸溶液中,經(jīng)水解、精制得咪達那新。結(jié)果 該合成工藝總收率為40.2%,終產(chǎn)物質(zhì)量分數(shù)為99.9%。結(jié)論 工藝改進后,簡化了操作過程,提高了咪達那新的收率。
[Key word]
[Abstract]
Objective To study the synthetic technology of imidafenacin. Methods Using 1,2-dibromomethane as the starting material, 4-bromo-2,2-diphenylbutyronitrile (1) was obtained after the phase transfer reaction with diphenylacetonitrile; compound 1 was then condensed with 2-methylimidazole in the presence of triethylamine in hot DMF-DMSO to obtain 4-(2-methyl-1-imidazolyl)- 2,2-diphenylbutyronitrile (2). Imidafenacin was obtained according to the hydrolysis of compound 2 in the presence of 70% sulfuric acid. Results The total yield by the synthetic process was 40.2%, and the purity of imidafenacin was 99.9%. Conclusion After the improvement of the process, the operating process is simplified and the yield of imidafenacin is improved.
[中圖分類號]
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