反应详情

温度

0 °C

To a solution of 1.81 g (12.81 mmol) nitrosylsulfuric acid in 1.5 ml water at 0° C. under nitrogene, was added dropwise a suspension of 463 mg (1.423 mmol) 2-benzyloxy-6-methoxy-4-trifluoromethyl-benzamide in 2.9 ml dichloromethane. The reaction mixture was stirred at 0° C. for 4 hours. The reaction mixture was poured over ice and extracted with dichloromethane. The combined organic layers were dried over sodium sulfate, filtered and evaporated. The crude solid was purified with flash column chromatography on silica (20 g) eluting with a gradient formed from n-heptane and ethyl acetate (0%=>100% in 15 minutes) to provide 431 mg (y: 64.9% yield) of the title compound as a white solid. MS (m/e): 325.1 (M−H)

1. additionThe reaction mixture was poured over ice
2. extractionextracted with dichloromethane
3. dry with materialThe combined organic layers were dried over sodium sulfate
4. filtrationfiltered
5. customevaporated
6. customThe crude solid was purified with flash column chromatography on silica (20 g)
7. washeluting with a gradient
8. customformed from n-heptane and ethyl acetate (0%=>100% in 15 minutes)