反应详情

Diethylaminotrimethylsilane (29.06 g, 0.2 mol) was added dropwise to a solution of 12.5 mL (0.1 mol) of diethylaminosulfur trifluoride in 75 mL of acetonitrile at 25°. The reaction mixture was stirred overnight, and then saturated with carbonyl fluoride. Evaporation of the solvent under reduced pressure gave 30.3 g (91%) of the trifluoromethoxide: mp 85°-95°; 1H NMR (CD3CN) δ1.21 ppm (t, J=7H, 9H), 3.29 ppm (q, J=7 Hz, 6H); 19F NMR (CD3CN) δ-20.8 ppm. Anal. Calcd. for C13H30F3N3OS: C, 46.83; H, 9.07; F, 17.07; N, 12.60. Found: C, 46.53; H, 9.17; F, 17.25; N, 12.55.

1. customEvaporation of the solvent under reduced pressure