J. Org. Chem. 1986, 51, 326-332
326
(0.40 mol) of 2,2,2-trifluoroethyl trifluoroacetate, and 50 g (0.50 mol) of TFE was shaken at ambient temperature for 8 h. The volatiles were removed from the reaction mixture under reduced pressure to give a viscous residue which was treated with 400 mL of water and 200 mL of concentrated H2S04. The mixture was stirred at 25 °C for 3 days and then at 70-80 °C for 3 days. The mixture was continuously extracted with ether for 12 h and the extract was distilled to a head temperature of 66 °C to remove the volatiles. The residual crude acid (118 g) was stirred with 100 g (1.0 mol) and 2,2,2-trifluoroethanol and 150 mL of concentrated H2S04 for 3 days. The mixture was distilled to give
179.4 g of
liquid, bp
