合成3,4-二氟苯基异硫氰酸酯的绿色工艺

目的开发出一条新的环保工艺代替文献报导的卡卢扎反应,制备3,4-二氟苯基异硫氰酸酯。方法3,4-二氟苯胺与二硫化碳在氢氧化钠水溶液中反应1 h,制得新的中间体N,N-二（3,4-二氟苯基）硫脲,后者在醋酐中加热分解得到1分子的目标物和1分子3,4-二氟苯基乙酰胺,副产物可以回收再使用。结果得到3,4-二氟苯基异硫氰酸酯,收率为40%。结论新工艺无需使用氯甲酸乙酯,避免了原工艺长时间的低温控制。

Environmental novel synthesis technology for 3,4-diflorophenyl isothiocyanate

Objective To develop an environmental new preparation technology for 3,4-diflorophenyl isothiocyanate, an important immediate of prulifolxacin.Methods 3,4-diflouroalline was condensed with CS2 in NaOH to prepare N,N-bis3,4-diflourphenyl] thiourea which was acidolysis in hot (AcO)2O to give the tittle compound, the main vice-product 3,4-diflouroalline acetate can be recycled. N,N-bis3,4-diflourphenyl]thiourea was a novel intermediate.Results Obtained 3,4-diflourphenyl isothiocyanate with overall yield of 40%.Conclusion An environmental new preparation technology is studied in which ethyl formate chloride is substituted, and conditions such as long-time and low-temperature are not necessary.