摘要
先以3-三氟甲基-4-溴苯胺(Ⅱ)为原料,与亚铁氰化钾发生氰基取代反应生成3-三氟甲基-4-氰基苯胺(Ⅲ);再以水为介质、DMF为有机溶剂,化合物Ⅲ与二硫化碳反应得到中间体3-三氟甲基-4-氰基苯基二硫代甲酸盐(Ⅳ);最后在三聚氯氰的作用下脱硫得到目标产物4-异硫氰基-2-(三氟甲基)苯甲腈(Ⅰ),反应总收率70.8%。目标产物的结构经1 HNMR和HPLC确证,HPLC纯度达99.5%。
Using 3-trifluoromethyl-4-bromoaniline（Ⅱ）as a starting material,3-trifluoromethyl-4-cyano-aniline（Ⅲ）was obtained by cyano substitution reaction with potassium ferrocyanide.Then using water as media,intermediate 3-trifluoromethyl-4-cyano-phenyldithiocarboxylic formate（Ⅳ）was obtained by reaction of the compoundⅢ with carbon disulfide in presence of organic solvent DMF.Finally,the target compound 4-isothiocyanato-2-（trifluoromethyl）benzonitrile（Ⅰ）was obtained by desulfurization of cyanuric chloride.The total yield was 70.8%.The structure of target compound was confirmed by 1 HNMR and HPLC,and the HPLC purity reached 99.5%.
出处
《化学与生物工程》
CAS
2016年第4期33-36,共4页
Chemistry & Bioengineering
基金
湖北省自然科学基金重点项目(2011CDA048)
武汉工程大学研究生创新基金资助项目(CX2014006)
