反应详情

To an ice-cold solution of morpholinosulfur trifluoride (4.9 mL, 40 mmol) in anhydrous diethyl ether (100 mL) is added, dropwise and under nitrogen, a solution of borontrifluoride etherate (4.2 mL, 40 mmol) in anhydrous diethyl ether (25 mL) over a period of 60 min, while keeping the reaction temperature below 5° C. The resulting suspension is stirred for an additional hour at the same temperature, then allowed to warm to room temperature and filtered under a blanket of nitrogen. The solid material is rinsed twice with diethyl ether (2×50 mL), then dried under vacuum to provide morpholinodifluorosulfinium tetrafluoroborate (7.3 g, 75%) as a white solid; m.p. 122-125° C.; 1H NMR (CD3CN, 300 MHz) δ 3.90-3.85 (m, 8H); 19F NMR (CD3CN, 282 MHz) δ 10.2 (s, 2F), −151.3 (s, 4F); 13C NMR (CD3CN, 75 MHz) δ 65.7, 48.3 (br).

1. customthe reaction temperature below 5° C
2. filtrationfiltered under a blanket of nitrogen
3. washThe solid material is rinsed twice with diethyl ether (2×50 mL)
4. customdried under vacuum