反应详情

Potassium peroxomonosulfate (Oxone, 67.2 mg, 0.110 mmol) was added to a stirring solution of 2-(4-chlorophenyl)-N-[5-({7-[(methylthio)methyl]-7H-pyrrolo[2,3-d]pyrimidin-5-yl}carbonyl)pyridin-3-yl]acetamide (Example 313, 25.0 mg, 0.055 mmol) in methanol (1.0 mL) and water (0.25 mL) at 0° C. After 1 hour, the reaction was allowed to warm to room temperature and stirred for 24 hours. The reaction mixture was cooled to 0° C. and sodium metabisulfite (0.5M, 1 ml) was added. The reaction mixture was evaporated under reduced pressure to remove the methanol. Water (3 mL) was added to the mixture and it was extracted with EtOAc (3×5 mL). The combined organic fractions were washed with water (5 mL), brine (5 mL), dried over magnesium sulfate the solvent was removed under reduced pressure to give the crude product as an off-white solid.

1. temperatureThe reaction mixture was cooled to 0° C.
2. customThe reaction mixture was evaporated under reduced pressure
3. customto remove the methanol
4. additionWater (3 mL) was added to the mixture and it
5. extractionwas extracted with EtOAc (3×5 mL)
6. washThe combined organic fractions were washed with water (5 mL), brine (5 mL)
7. dry with materialdried over magnesium sulfate the solvent
8. customwas removed under reduced pressure