反应详情

To a stirred solution of {4-[3-[3-(2-chloro-benzylamino)-phenyl]-1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrazolo[3,4-d]pyrimidin-6-ylamino]-cyclohexyl}-carbamic acid tert-butyl ester (110 mg, 0.162 mmol) in dichloromethane (3 mL) was added TFA (3 mL) at room temperature. The resulting mixture was stirred for another four hours at this temperature. The solvent was evaporated under reduced pressure and the residue was treated with saturated aqueous NaHCO3 (5 mL) and extracted with EtOAc (30 mL). The organic phase was washed with brine (5 mL) and dried to give crude product. It was purified by prep-HPLC to give N-{3-[3-(2-chloro-benzylamino)-phenyl]-1H-pyrazolo[3,4-d]pyrimidin-6-yl}-cyclohexane-1,4-diamine as solid. (Yield 15 mg, 21%).

1. customThe solvent was evaporated under reduced pressure
2. additionthe residue was treated with saturated aqueous NaHCO3 (5 mL)
3. extractionextracted with EtOAc (30 mL)
4. washThe organic phase was washed with brine (5 mL)
5. customdried
6. customto give crude product
7. customIt was purified by prep-HPLC