2-氯-4-硝基-α,α,α-三氟甲氧基苯的氟化反应研究

Study of the Fluorination of 2-Chloro 4-nitrotrifluoromethoxybenzene

研究了 2 氯 4 硝基 α ,α ,α 三氟甲氧基苯 (CNTFMB)的氟化反应 ,考察了溶剂、相转移催化剂聚乙二醇 (PEG60 0 0 )、KF用量等因素对反应的影响。经实验确定了反应的最佳工艺条件为 :n(CNTFMB)∶n(KF) =1 0∶1 4,CNTFMB的质量 (g)与溶剂DMF的体积 (mL)之比为 1∶3,n(PEG60 0 0 )∶n (CNTFMB) =0 5∶10 0 0 ,反应温度 135℃。在此条件下 ,2 氟 4 硝基 α ,α ,α 三氟甲氧基苯 (FNTFMB)的收率为 85 % ,产品纯度w (FNTFMB) =95 %。

The fluorination of 2-chloro-4-nitro-α, α, α-trifluoromethoxybenzene (CNTFMB) was studied in DMF using spray-dried KF as fluorinating agent and polyetlhyleneglycol PEG6000 as phase transfer catalyst. The optimum reaction conditions were determined: n (CNTFMB): n (KF) = 1.00: 1.40, quantity (g) of CNTFMB: volume (mL) of DMF = 1: 3, n (PEG6000): n (CNTFMB) = 0.5:100.0, t = 135 °C. Yield of 2-fluoro-4-nitro-α, α, α-trifluoromethoxybenzene was over 85% and its purity was more than 95%.