反应详情

温度

45 °C

To a mixture of (S)-tert-butyl 3-(4-amino-3-iodo-1H-pyrazolo[3,4-d]pyrimidin-1-yl)-1-piperidinecarboxylate (3.4 g, 0.0077 mol) in acetone (80 mL) was added an aqueous 6N solution of hydrogen chloride (20 mL) at room temperature. The mixture was stirred at 45° C. for 4 hours, then at room temperature for 18 hours. Acetone was removed under reduced pressure, and the aqueous layer was washed with toluene (2×20 mL) and dichloromethane (2×20 mL). The aqueous layer was basified with an aqueous 5N solution of sodium hydroxide (25 mL) at 0° C. The aqueous layers were concentrated to dryness, and the residue was purified by RP-HPLC (Hypersilprep HS C18, 8 μm, 250×21.1 mm; 2%-30% over 15 min with 0.1 M ammonium acetate, 21 mL/min) to yield (S)-3-iodo-1-(3-piperidyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine acetate (0.75 g, 0.0019 mol).

1. waitat room temperature for 18 hours
2. customAcetone was removed under reduced pressure
3. washthe aqueous layer was washed with toluene (2×20 mL) and dichloromethane (2×20 mL)
4. customwas basified with an aqueous 5N solution of sodium hydroxide (25 mL) at 0° C
5. concentrationThe aqueous layers were concentrated to dryness
6. customthe residue was purified by RP-HPLC (Hypersilprep HS C18, 8 μm, 250×21.1 mm; 2%-30% over 15 min with 0.1 M ammonium acetate, 21 mL/min)