二苯基硫脲的合成与分析

Synthesis and Analysis of N,N'-Diphenyl Thiourea

探讨了一种合成二苯基硫脲(DPTU)的新方法.以酸性树脂作为催化剂、苯胺和二硫化碳作为反应物在温和条件下选择性地合成了DPTU,考察了催化剂用量和反应时间对产物收率的影响.结果表明:酸性树脂对本反应有显著促进作用;反应4h内DPTU收率随反应时间迅速增加,4h后则增加缓慢;用4g催化剂、9.1mL苯胺和12mL CS2(摩尔比为1:2)在回流温度下反应6h,DPTU的收率达82.7%,选择性为100%.用GC/MS,HPLC/MS,FTIR,UV和1H NMR分析了合成的DPTU.

A new approach to the synthesis of N,N'-diphenyl thiourea (DPTU) was investigated. DPTU was selectively synthesized using aniline and CS2 as reactants and acidic resin as catalyst under mild conditions. The effects of catalyst feed and reaction time on DPTU yield were examined. The results show that the acidic resin remarkably promotes the reaction; The DPTU yield increases rapidly with reaction time being less than 4 h, but it increases slowly after 4 h reaction; DPTU yield and selectivity may reach 82. 7% and 100%, respectively, for the reaction of 9. 1 mL of aniline with 12 mL of CS2 using 4 g of acidic resin as catalyst at reflux temperature. The resulting DPTU was analyzed with GC/MS, HPLC/MS, FTIR, UV and H NMR.