摘要
研究和优化了以3 溴 4 氟甲苯(Ⅲ)和苯酚(Ⅰ)为原料,经Ullmann偶联缩合反应合成对氟间苯氧基甲苯(Ⅳ)的方法。最佳实验条件是x(CuO)=15%为催化剂,n〔苯酚钠(Ⅱ)〕∶n(Ⅲ)=3∶1,DMA作溶剂,在160～165℃反应5h,Ⅳ的产率可达88%,气相色谱纯度w(Ⅳ)=98 2%。Ⅳ的结构经1HNMR,IR,元素分析和ESI-MS证实。
4-Fluoro-3-phenoxytoluene (Ⅳ) was synthesized by Ullmann coupling reaction of 3-bromo-4-fluorotoluene (Ⅲ) and phenol(Ⅰ).When the molar ratio of PhONa (Ⅱ) to Ⅲ was 3∶1 with 15%(mol) of CuO as catalyst and DMA as solvent,the reaction ran at 160～165 ℃ for 5 h to give Ⅳ in 88% yield with purity w(Ⅳ)=98.2% by GC.The structure of Ⅳ was confirmed by elementary analysis,~1HNMR,IR,and MS.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2004年第5期395-397,共3页
Fine Chemicals
基金
河南省自然科学基金资助项目[2001(0111030500)]
