摘要
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。
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 CSz in NaOH to prepare N, N-bis [3, 4-diflourphenyl] thiourea which was acidolysis in hot （AcO）2O to give the tittle compound, the main viceproduct 3, 4-diflouroalline acetate can be recycled. N, N-bis [3, 4-diflourphenyt] 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.
出处
《中南药学》
CAS
2009年第7期521-522,共2页
Central South Pharmacy
