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对康布瑞汀磷酸酯二钠盐的合成工艺进行优化.确定了以3,4,5-三甲氧基苯甲醛为原料,经还原、溴代、成鏻盐合成中间体3,4,5-三甲氧基苄溴三苯基鏻盐;鏻盐与3-三苯甲氧基-4-甲氧基苯甲醛经Wittig反应、脱三苯甲基保护基、与亚磷酸二苄酯成酯、脱苄基成钠盐得到康布瑞汀磷酸酯二钠盐的方法.所得康布瑞汀磷酸酯二钠盐(1),HPLC纯度达99.5%.总收率为43.0%.经优化后的工艺原料价廉易得,操作简便,成本低廉,适合于工业化生产.
The synthesis process of combretastatin phosphate disodium salt was optimized.It was confirmed that 3,4,5-trimethoxybenzaldehyde was used as the raw material to synthesize intermediate 3,4,5 - trimethoxybenzyl bromide triphenylphosphonium salt; phosphonium salt and 3-trityloxy-4-methoxybenzaldehyde by Wittig reaction, detritylic protection group, and dibenzyl phosphite ester , Debenzylation into sodium salt to obtain the content of combretastatin phosphate disodium salt, the obtained combretastatin phosphate disodium salt (1) with an HPLC purity of 99.5% and an overall yield of 43.0%. The optimized Process raw materials cheap easy to get, easy to operate, low cost, suitable for industrial production.