【摘要】 在KOH和K2CO3存在下,通过对氯三氟甲苯(PCTFB)和2,5-二甲基苯酚在N-甲基吡咯烷酮(NMP)中的缩合反应制得了2-(4-三氟甲基苯氧基)对二甲苯(TFDMB),该步最佳的反应条件为:PCTFB与2,5-二甲基苯酚的摩尔比为1∶1.2,反应时间为8 h,反应温度为140~190℃,TFDMB的产率达93.7%.TFDMB继而用KMnO4作氧化剂分别在吡啶、NaOH的水溶液中经两步氧化制得关键中间体2-(4-三氟甲基苯氧基)对苯二甲酸(TFPA),产率为75%;再将TFPA和氯化亚砜反应以92%的产率合成了聚合单体2-(4-三氟甲基苯氧基)对苯二甲酰氯(TFTPC),三步总收率为64.6%.更多还原

【Abstract】 2-（4-Trifluoromethylphenoxy）paradimethylbenzene（TFDMB） was prepared by the condensation of 2,5-dimethylphenol and 1-chloro-4-trifluoromethyl benzene in NMP in the presence of KOH and K₂CO₃.The optimum reaction conditions was obtained as follows: 1-chloro-4-trifluoromethyl benzene/2,5-dimethylphenol 1∶1.2,reaction temperature 140～190 ℃,reaction time 18 h.The yield of TFDMB reached 93.7%.TFDMB was subsequently oxidated into key intermediate,2-（4-trifluoromethylphenoxy）paraphthalic acid（TFPA） with 75% yield in the presence of KMnO₄ in aqueous solution of pyridine and sodium hydroxide in two step,respectively.And then reaction of TFPA with sulfur oxychloride yielded polymerization-grade monomer 2-（4-trifluoromethylphenoxy）terephthalyl chloride（TFTPC） in 92 % yields.The overall yield of the three-step reaction for TFTPC was 64.6%.更多还原