反应详情

温度

40 °C

A stirred solution of (3R,4R)-3-{4-Methyl-3-[methyl-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-amino]-piperidin-1-yl}-3-oxo-propionitrile (230 mg/0.74 mmol) dissolved in 23 mL of acetone was heated to 40° C. To this solution was added 155 mg (0.81 mmol) of finely ground citric acid. The resulting mixture stirred at 40° C. for 2 hours, then at 30° C. for 4 hours followed by stirring at room temperature for an additional 18 hours. At this point, the solids were collected by filtration, washed with acetone and dried in vacuo affording 280 mg (75%) of the title compound as a white crystalline solid.

1. waitat 30° C. for 4 hours followed
2. stirringby stirring at room temperature for an additional 18 hours
3. filtrationAt this point, the solids were collected by filtration
4. washwashed with acetone
5. customdried in vacuo