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报道了一种合成噻螨酮关键中间体——反式-5-(4-氯苯基)-4-甲基-2-氧代噻唑烷酮的方法。以赤式-1-对氯苯基-2-氨基丙醇盐酸盐和二硫化碳为原料,在130℃下直接环合得到反式5-(4-氯苯基)-4-甲基-2-氧代噻唑烷酮,收率82%,色谱纯度99%;再经双氧水氧化得到噻螨酮关键中间体,收率84%,色谱纯度95%。该工艺流程经两步合成得到目标产物,简化了操作步骤,缩短了反应时间,避免了酸性废水的排放,符合绿色化工的要求。
A method for synthesizing the key intermediate of hesperidone, trans-5- (4-chlorophenyl) -4-methyl-2-oxothiazolidinone, was reported. Starting from erythro-1-p-chlorophenyl-2-aminopropanol hydrochloride and carbon disulfide, cyclization directly at 130 ° C gave trans 5- (4-chlorophenyl) - oxothiazolidinone, yield 82%, chromatographic purity 99%; and then oxidized by hydrogen peroxide to obtain the key intermediate hesperidin, 84% yield, 95% chromatographic purity. The process is synthesized by two steps to obtain the target product, which simplifies the operation steps, shortens the reaction time and avoids the discharge of acidic waste water, and meets the requirements of the green chemical industry.