CAJ | 학술논문

合成考尼伐坦关键中间体2-甲基-6-(4-甲基苯磺酰基)-1,4,5,6-四氢咪唑[4,5-d][1]苯并氮杂卓并对其工艺优化。以氨茴酸甲酯为起始原料,经保护、烃化、环合、脱羧、溴化、烃化并缩合共六步反应合成考尼伐坦关键中间体。所得的目标化合物经核磁共振氢谱、质谱确认,总收率达49．06%。该关键中间体合成方法和工艺改进后,所用原料价格便宜、反应条件温和、反应周期缩短、产率提高,更加适合于工业化生产。
합성고니벌탄관건중간체2-갑기-6-(4-갑기분광선기)-1,4,5,6-사경미서[4,5-d][1]분병담잡탁병대기공예우화。이안회산갑지위기시원료,경보호、경화、배합、탈최、추화、경화병축합공륙보반응합성고니벌탄관건중간체。소득적목표화합물경핵자공진경보、질보학인,총수솔체49．06%。해관건중간체합성방법화공예개진후,소용원료개격편의、반응조건온화、반응주기축단、산솔제고,경가괄합우공업화생산。
The key intermediate of Conivaptan,2-methyl-6-tosyl-1,4,5,6-tetrahydrobenzo[b]imidazo[4,5-d]azepine,which was from methyl anthranilate in six steps including protection,alkylation,cyclization,decarboxylation,bromination,alkylation and con-densation etc was synthesized. The structure of intermediate was characterized based on MS and 1 H NMR. The overall yield of the synthetic route was 49. 06%. An optimal process was provided that free from problems other synthesis routes encountered,and could be ready to scale-up production.