2(3H)-Benzoxazolone → 6-Benzoxazolesulfonyl chloride, 2,3-dihydro-2-oxo-
반응식
[CH:1]1[CH:2]=[CH:3][C:4]2[O:10][C:8](=[O:9])[NH:7][C:5]=2[CH:6]=1.[Cl:11][S:12](O)(=[O:14])=[O:13]>>[O:9]=[C:8]1[NH:7][C:5]2[CH:6]=[CH:1][C:2]([S:12]([Cl:11])(=[O:14])=[O:13])=[CH:3][C:4]=2[O:10]1참가 물질
3
반응 조건
- 온도
- 25 °C
실험 절차
Benzoxazolinone (13.5 g, 0.1 mol) was added slowly to a 0° C. solution of chlorosulfonic acid (33.29 mL, 5 equivalents). The reaction was warmed to 25° C. and stirred for 0.5 h, heated to 60° C. for 3 h. The reaction was cooled to 25° C., poured into ice, filtered, and rinsed with water. The resulting white solid was redissolved in 500 mL of diethyl ether and washed with water (2×), dried over Na2SO4, filtered and concentrated to 100 mL volume. Hexane was added (100 mL) and the white precipitate was filtered and placed under vacuum to yield 17 g (73%) of the title compound.