反应详情

温度

45 °C

The crude tert-butyl 4-(4-amino-3-iodo-1H-pyrazolo[3,4-d]pyrimidin-1-yl)-1-piperidinecarboxylate (69.4 g, 156.30 mmol) was dissolved in acetone (900 mL) and 6N aqueous hydrochloric acid (300 mL) was slowly added dropwise. The reaction was then heated at 45° C. which yielded a precipitate. After 1.5 hours, the precipitate was collected by vacuum filtration, washed with minimal acetone and dried on the lyophilizer to yield 3-iodo-1-(4-piperidyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine dihydrochloride salt as a yellow solid (16.61 g, 39.8 mmol). HPLC-RT: 6.16 min. (flow rate: 1 mL/min λ=254 nm Gradient: 5% to 85% acetonitrile/0.1M aqueous ammonium acetate gradient over 20 min.; Deltapak C18, 300A, 5 μm, 150×3.9 mm column); m/z (MH+)=345.0.

1. customyielded a precipitate
2. filtrationthe precipitate was collected by vacuum filtration
3. washwashed with minimal acetone
4. customdried on the lyophilizer