反应详情

温度

0 °C

1-(1,4-dioxaspiro[4.5]dec-8-yl)-3-iodo-1H-pyrazolo[3,4-d]pyrimidin-4-ylamine (intermediate N) (13.12 g, 32.7 mmol) was suspended in acetone (240 mL) and the mixture was cooled to 0° C. Added aqueous 5 N HCl (200 mL) dropwise, keeping the temperature less than 4° C. during the addition. After the addition was complete the mixture was allowed to come to ambient temperature and stirred for 18 hours. The remaining solid was removed by filtration, and the filtrate was neutralized with saturated aqueous sodium bicarbonate. The precipitate was collected by filtration and washed with water and dried in vacuo to give 4-(4-amino-3-iodo-1H-pyrazolo[3,4-d]pyrimidin-1-yl)-1-cyclohexanone (8.20 g, 32.8 mmol): 1H NMR (DMSO-d6, 400 MHz) 8.23 (s, 1H), 5.18 (m, 1H), 2.64-2.73 (m, 2H), 2.26-2.37 (m, 4H), 2.17-2.30 (m, 2H).

1. customthe temperature less than 4° C.
2. additionduring the addition
3. additionAfter the addition
4. customto come to ambient temperature
5. customThe remaining solid was removed by filtration
6. filtrationThe precipitate was collected by filtration
7. washwashed with water
8. customdried in vacuo