2-氟-6-三氟甲基苯磺酰氯的合成工艺研究

以间氟三氟甲苯为原料,采用邻位锂化法合成了2-氟-6-三氟甲基苯磺酰氯。通过单因素试验确定了反应的工艺条件。优化后的反应条件为:锂化反应以n-BuLi作为反应的碱,锂化反应温度-50℃,n(间氟三氟甲苯)∶n(n-BuLi)=1∶1;酰氯化反应温度-30℃,n(间氟三氟甲苯)∶n(SO2Cl2)=1.0∶1.2。经优化后,反应收率为86.8%,气相色谱检测产品含量为98.2%。该方法具有收率高、操作简单的特点,适合于工业生产。

Study on the Synthesis of 2-Fluoro-6-trifluoromethyl-benzenesulfonyl Chloride

2-Fluoro-6-trifluoromethylbenzenesulfonyl chloride was synthesized from m-fluorotrifluoro-methylbenzene by ortho lithiation. The reaction conditions were determined by single factor experiment. The optimized reaction conditions are as follows: n-BuLi is the base of lithium reaction, the temperature of lithium reaction is-50 ℃, n(m-fluorotrifluoromethylbenzene) ∶n(n-BuLi)=1 ∶1;the temperature of acyl chlorination is-30 ℃, n(m-fluorotrifluoromethylbenzene) ∶n(SO2Cl2)=1.0 ∶1.2. After optimization, the yield was 86.8%, and the content of product was 98.2% by gas chromatography. This method has the characteristics of high yield and simple operation, and is suitable for industrial production.