反应详情

温度

100 °C

Thioxanthene, 29 (2.9 g, 14.6 mmol) was dissolved in glacial acetic acid (90 mL). While under argon, the solution was treated with hydrogen peroxide (6.12 mL, 62.9 mmol of a 35% by wt water solution) and the reaction stirred at 100° C. for 1.5 hr. The reaction was cooled to room temperature, poured into water (250 mL), stirred 0.5 hrs and filtered to give a white solid. The solid was dissolved in CH2Cl2, washed with 5% sodium bisulfite (aq), dried over Na2SO4, filtered and concentrated to dryness in vacuo. Treatment of the resulting oil with methanol gave the title compound as a white solid.

1. temperatureThe reaction was cooled to room temperature
2. stirringstirred 0.5 hrs
3. filtrationfiltered
4. customto give a white solid
5. washwashed with 5% sodium bisulfite (aq)
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated to dryness in vacuo