反应详情

温度

0 °C

A solution of 4-methyl-3-(1-(2-methyl-4-(methylthio)phenyl)phthalazin-6-yl)benzamide (170 mg, 0.43 mmol, Method D) in 2 mL of 10/1 methanol/H2O at 0° C. was treated with oxone (262 mg, 0.43 mmol). The mixture stirred at 0° C. for 1 h and then warmed up to RT for 1 h. The reaction was quenched with 20 mL sodium sulfite (sat.) and extracted with 10% MeOH in dichloromethane. The combined organic layers were dried over anhydrous sodium sulfate, filtered and concentrated. The crude material was purified by HPLC to give 4-methyl-3-(1-(2-methyl-4-(methylsulfonyl)phenyl)phthalazin-6-yl)benzamide as a white solid. Found MS (ES+)=432.1 (M+H+).

1. temperaturewarmed up to RT for 1 h
2. customThe reaction was quenched with 20 mL sodium sulfite (sat.)
3. extractionextracted with 10% MeOH in dichloromethane
4. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude material was purified by HPLC