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2-[(4-甲基苯磺酰基)胺基]苯甲酸甲酯(6)与4-氯丁腈在相转移催化剂聚乙二醇-400和混合碱(KOH+K_2CO_3)作用下发生N-烷基化反应得2-[N-(3-氰基丙基)-4-甲基苯磺酰胺基]苯甲酸甲酯,经缩合关环、脱氰基、溴代、与盐酸乙脒缩合关环、脱磺酰基得2-甲基-1,4,5,6-四氢咪唑并[4,5-d][1]苯并氮?(5)。另用2-苯基苯甲酸与4-氨基苯甲酸在N,N’-羰基二咪唑(CDI)作用下发生酰胺化反应得4-(2-苯基苯甲酰胺基)苯甲酸,与5在CDI作用下经酰胺化、成盐反应得盐酸考尼伐坦,总收率37.6%(以6计)。
The reaction of methyl 2 - [(4-methylphenylsulfonyl) amino] benzoate (6) with 4-chlorobutyronitrile under the action of phase transfer catalyst of polyethylene glycol-400 and mixed alkali (KOH + K 2 CO 3) - alkylation to give methyl 2- [N- (3-cyanopropyl) -4-methylphenylsulfonamido] benzoate, condensation ring closure, decyano, bromo, and acetamidine hydrochloride Condensation ring closure, desulfonyl to give 2-methyl-1,4,5,6-tetrahydroimidazo [4,5-d] [1] benzazepine (5). In addition, 4- (2-phenylbenzamido) benzoic acid was obtained by amidation of 2-phenylbenzoic acid and 4-aminobenzoic acid under the action of N, N’-carbonyldiimidazole (CDI) Under the action of CDI amidation, salting reaction to be conivalent hydrochloride, the total yield of 37.6% (in 6 dollars).