反应详情

In a dry box, methyl chloroformate (219 mL, 268 g, 2.84 mol) was added slowly to a solution containing 2,2,2-trifluoroethanol (233.5 g, 2.335 mol), pyridine (225 g), and dichloromethane (1.2 L, anhydrous) at −10° C. to 30° C. (the dichloromethane was cooled in a freezer before use), with magnetic stirring. The reaction mixture was stirred at room temperature in the dry box overnight. The reaction mixture was then taken out of the dry box, and was washed with 5% HCl (300 mL), followed by 3 washes with 50 mL portions of 5% HCl, one wash with 5% sodium carbonate (100 mL), and 2 washes with 100 mL portions of brine. The organic phase was then dried over anhydrous sodium sulfate. Dichloromethane was removed by rotary evaporation. The residue liquid was distilled with a spinner band column, yielding 185.4 g (46% yield) of pure methyl 2,2,2-trifluoroethyl carbonate, also referred to herein as “FS-D”. NMR analysis data were consistent with literature values (U.S. Pat. No. 5,659,062).

1. temperaturewas cooled in a freezer before use), with magnetic stirring
2. washwas washed with 5% HCl (300 mL)
3. washwash with 5% sodium carbonate (100 mL), and 2
4. dry with materialThe organic phase was then dried over anhydrous sodium sulfate
5. customDichloromethane was removed by rotary evaporation
6. distillationThe residue liquid was distilled with a spinner band column