反应详情

1-{2-cyano-1-[4-(7-[2-(trimethylsilyl)ethoxy]methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-pyrazol-1-yl]ethyl}cyclopropanecarbonitrile (48 mg, 0.11 mmol) was stirred in a mixture of DCM (3 mL) and TFA (2 mL) for 3 hours. The solvents were removed in vacuo and the residue was re-dissolved in THF (3 mL). 6N NaOH (2 mL) was added and the resulting mixture was stirred at ambient temperature for 3 hours. The crude reaction mixture was partitioned between ethyl acetate and water. The layers were separated and the organic layer was dried over sodium sulfate and the solvent was removed in vacuo. Purification via preparative-HPLC/MS (C18 eluting with a gradient of H2O and ACN containing 0.1% TFA) afforded product (20 mg, 43%).

1. customThe solvents were removed in vacuo
2. dissolutionthe residue was re-dissolved in THF (3 mL)
3. addition6N NaOH (2 mL) was added
4. customThe crude reaction mixture
5. customwas partitioned between ethyl acetate and water
6. customThe layers were separated
7. dry with materialthe organic layer was dried over sodium sulfate
8. customthe solvent was removed in vacuo
9. customPurification via preparative-HPLC/MS (C18
10. washeluting with a gradient of H2O and ACN containing 0.1% TFA)