水体系中硫代氯甲酸苯酯的无碱合成

摘要

以H 2 O/CHCl3为混合溶剂,苯酚钠和CSCl 2在无碱条件下反应得到硫代氯甲酸苯酯,收率85％.考察了碱、溶剂、原料配比、反应时间、反应温度和反应规模等因素对产物收率的影响,得到了最佳的反应条件:n(苯酚钠):n(CSCl 2)=1:1.2,室温反应5 h,V(H 2 O):V(CHCl 3)=1:1.反应规模可扩大到500 g,收率81％,具有潜在的应用价值.%The synthesis of phenoxythiocarbonyl chloride in aqueous solvent under base-free conditions was developed. The phenoxy-thiocarbonyl chloride was obtained starting from phenol sodium and CSCl2 in 85％ yield. The reaction conditions were optimized in the respect of bases,solvents,substrate ratio,reaction time,reaction temperature and reaction scales,and the optimized reaction con-ditions were:n(phenol sodium): n(CSCl 2 )= 1 : 1. 2,r. t. ,5 h,V(H 2 O): V(CHCl 3 )= 1 : 1. The yield was up to 81％ at 500 grams scale,which made this route more attractive for industrial application.