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[摘要]
目的 对咪达那新的合成工艺进行研究。方法 以二苯乙腈为起始原料,与1,2-二溴乙烷经相转移反应生成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–二甲基亚砜中与2-甲基咪唑反应,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,经水解、精制得咪达那新。结果 该合成工艺总收率为40.2%,终产物质量分数为99.9%。结论 工艺改进后,简化了操作过程,提高了咪达那新的收率。
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[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.
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