反应详情

To a cooled (0° C.) solution of 119 (1.24 g; 7.7 mmol) in anhydrous dichloromethane (38 mL) was added chlorosulfonic acid (0.61 mL; 9.24 mmol) dropwise (1 mL/minutes). The reaction mixture w as allowed to gradually warm to room temperature while stirring overnight. The reaction mixture was concentrated under reduced pressure. The resulting oil w as taken up in diisopropyl ether (10 mL) and aqueous hydrochloric acid (0.5 mL; 2N) then stirred vigorously at room temperature for 2 hours. The organic phase was separated and concentrated under reduced pressure to yield the desired compound as an amber oil (1.8 g).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. stirringaqueous hydrochloric acid (0.5 mL; 2N) then stirred vigorously at room temperature for 2 hours
3. customThe organic phase was separated
4. concentrationconcentrated under reduced pressure