噻螨酮的合成工艺

Synthesis of Hexythiazox

以赤式-1-对氯苯基-2-氨基丙醇为原料,经酯化反应,二硫化碳环合,双氧水氧化,最后与环己基异氰酸酯缩合得到噻螨酮。酯化中以氯磺酸代替浓硫酸作为反应试剂,提高了产率,缩短了反应时间;二硫化碳环合反应的最佳条件:硫酸酯II与二硫化碳的摩尔比为1∶3,反应温度55℃;双氧水氧化反应的最佳条件:硫酮III、双氧水、甲醇钠的摩尔比为1∶3.5∶3.5,反应温度30℃。产品含量97.8%,总收率达到77.6%。

Started from erythro-2-amino-1-（chloro-phenyl）-1-propanol, the hexythiazox was obtained via esterification, carbon disulfide cyclocondensation, hydrogen peroxide oxidation and condensation with cyclohexyl isocyanate. The reactive time was shorted and the yield was increased while concentrated sulfuric acid was substituted by chlorosulfonic acid as reagent in esterification. The optimum process conditions of carbon disulfide cyclocondensation and hydrogen peroxide oxidation were： n（sulfateⅡ） ：n（carbon disulfide）=1 ：3, reaction temperature 55 ℃, n（thioneⅢ）：n（hydrogen perxide）：n（sodium methylate）=1：3.5：3.5, reaction temperature 30 ℃. The content of the product was 97.8%, and the total yield was 77.6%.