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以柠檬酸为起始原料,在浓硫酸中氧化并脱去一个羧基,生成丙酮二羧酸,再通过酯化、环合、烷基化反应生成雷尼酸四甲酯,最后水解成盐得到雷尼酸锶,即2-[N,N-二(羧甲基)氨基]-3-氰基-4-羧甲基-噻吩-5-甲酸二锶盐。通过正交实验和单因素实验考察了影响前3步反应的诸多因素,确定最佳工艺条件,总收率达到37.9%。各中间体及目标产物的结构通过核磁共振氢谱、元素分析及X射线粉末衍射表征。
Citric acid as the starting material in the concentrated sulfuric acid oxidation and removal of a carboxyl group, to generate acetone dicarboxylic acid, and then by esterification, cyclization, alkylation reaction of methyl thiolate, the final hydrolysis salt Strontium ranelate, ie, 2- [N, N-bis (carboxymethyl) amino] -3-cyano-4-carboxymethyl-thiophene-5-carboxylate. Through orthogonal experiment and single factor experiment, the factors affecting the first three reaction steps were investigated and the optimum technological conditions were determined. The total yield reached 37.9%. The structure of each intermediate and target product was characterized by 1H nuclear magnetic resonance spectroscopy, elemental analysis and X-ray powder diffraction.