论文部分内容阅读
5-氯-2-硝基苯甲酸先还原、再酯化得到2-氨基-5-氯苯甲酸甲酯,然后经磺酰化、N-烷基化得5-氯-2-[N-(3-乙氧羰基丙基)-N-(对甲苯磺酰基)]氨基苯甲酸甲酯,再经Dieckmann缩合、在硫酸中同时脱羧和脱磺酰基得到托伐普坦关键中间体7-氯-5-氧代-2,3,4,5-四氢-1H-1-苯并氮,总收率约71%。
5-Chloro-2-nitrobenzoic acid is first reduced and then esterified to give methyl 2-amino-5-chlorobenzoate, which is then sulfonylated and N-alkylated to give 5-chloro-2- [N- (3-ethoxycarbonylpropyl) -N- (p-toluenesulfonyl)] aminobenzoate, which was then decarboxylated and de-sulfone in sulfuric acid to give the key intermediate of tolvaptan 7-chloro Oxo-2,3,4,5-tetrahydro-1H-1-benzazepine in a total yield of about 71%.