反应详情

To a solution of tert-butyl 4-(3-[4-amino-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-1-yl]-1-azetanylmethyl)-4-hydroxy-1-piperidinecarboxylate (0.090 g, 0.00016 mol) in dichloromethane (2 mL) was slowly added a 20% solution of trifluoroacetic acid in dichloromethane (10 mL) at 0° C. under an atmosphere of nitrogen. The mixture was warmed to room temperature and stirred for four hours. The solvent was removed under reduced pressure. An aqueous solution of 5 N sodium hydroxide was added to pH 11 at 0° C. The water phase was extracted with dichloromethane (2×30 mL). The combined organic extracts were washed with water (1×60 mL) and brine (1×60 mL) and dried over sodium sulfate. The solvent was removed under reduced pressure to yield 4-(3-[4-amino-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-1-yl]-1-azetanylmethyl)-4-piperidinol (0.045 g, 0.000096 mol).

1. customThe solvent was removed under reduced pressure
2. additionAn aqueous solution of 5 N sodium hydroxide was added to pH 11 at 0° C
3. extractionThe water phase was extracted with dichloromethane (2×30 mL)
4. washThe combined organic extracts were washed with water (1×60 mL) and brine (1×60 mL)
5. dry with materialdried over sodium sulfate
6. customThe solvent was removed under reduced pressure