【摘要】 以对甲苯磺酰氯为起始原料,经氯化、还原和烷基化3步反应,合成了玉米田高效除草剂磺草酮中间体3-氯-4-甲基苯甲砜。研究了反应温度、反应时间、原料配比和催化剂等因素对反应收率的影响。在最佳工艺条件下,即摩尔比分别是对甲苯磺酰氯∶三氯化锑为70∶1,三氯化锑∶碘为7∶1时,于75℃～80℃通氯反应3h,得3-氯-4-甲基苯磺酰氯;亚硫酸钠∶氯乙酸钠∶3-氯-4-甲基苯磺酰氯为1.1∶1.5∶1时,先于75℃～80℃还原反应4h,再于103℃～106℃回流反应20h,得3-氯-4-甲基苯甲砜,3步反应的总收率为91.2%,产物纯度为99.5%。更多还原

【Abstract】 3-Chloro-4-methyl-methylsulfonylbenzene,an intermediate of sulcotrione,was synthesized using 4-methylbenzenesulfonyl chloride as a primary material,following by chlorination,reduction and alkylation. The influ-ence on reaction temperature,reaction time,reactant ratio and catalyst was investigatd. The optimum reaction condi-tions are as follows: the chlorinating reaction was carried out at a molar ratio of 4-methylbenzenesulfonyl chloride/ antimony trichloride was 70∶1 and antimony trichloride/iodine was 7∶1 for 3 h at 75-80 °C. The reducting and alkylating reactions were carried out at a molar ratio of sodium sulfite/sodium choloacetate/3-chloro-4-methyl-benzenesulfonyl chloride was 1.1∶1.5∶1 for 4h at 75-80 °C and for 20 h at 103-106 °C respectively with a total yield of 91.2% and a purity of 99.5% in the preparation of 3-chloro-4-methyl-methylsulfonylbenzene.更多还原