反应详情

Methyl chloroformate (130 mL, 159 g, 1.68 mol) was added slowly over a period of 3 hours to a solution of 2,2,3,3-tetrafluoropropanol (132 g, 1.00 mol) in pyridine (300 mL, anhydrous) at −10° C. to 0° C. with magnetic stirring. The reaction mixture was stirred at room temperature overnight. Then, the reaction mixture was mixed with 5% HCl (500 mL) and approximately 50 g of ice, and the resulting mixture was extracted three times with 300 mL portions of ether. The combined organic layer was washed three times with 100 mL portions of 5% HCl, followed by two washes with 100 mL portions of 5% sodium carbonate. The organic phase was then dried over anhydrous sodium sulfate. Ether was removed by rotary evaporation. The crude product (approximately 200 g) was distilled, yielding 166 g (87% yield) of pure methyl 2,2,3,3-tetrafluoropropyl carbonate, also referred to herein as “FS-C”. NMR analysis data were consistent with the literature values as reported in U.S. Pat. No. 5,659,062.

1. extractionthe resulting mixture was extracted three times with 300 mL portions of ether
2. washThe combined organic layer was washed three times with 100 mL portions of 5% HCl
3. dry with materialThe organic phase was then dried over anhydrous sodium sulfate
4. customEther was removed by rotary evaporation
5. distillationThe crude product (approximately 200 g) was distilled