反应详情

温度

25 °C

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.

1. temperatureheated to 60° C. for 3 h
2. temperatureThe reaction was cooled to 25° C.
3. additionpoured into ice
4. filtrationfiltered
5. washrinsed with water
6. dissolutionThe resulting white solid was redissolved in 500 mL of diethyl ether
7. washwashed with water (2×)
8. dry with materialdried over Na2SO4
9. filtrationfiltered
10. concentrationconcentrated to 100 mL volume
11. additionHexane was added (100 mL)
12. filtrationthe white precipitate was filtered