反应详情

To 1-(1,4-dioxaspiro[4.5]dec-8-yl)-3-(4-phenoxyphenyl)-pyrazolo[3,4d]pyrimidin4-ylamine (Compound 9) (4.2 g, 95 mmol) in acetone (200 mL) was added HCl (5N, 50 mL) dropwise. Stir at room temperature for 24 hrs. Evaporate the acetone and basify with NaOH (5N, 60 mL). Extract with EtOAc (3×200 mL). Dry, filter and evaporate to leave a solid which was triturated with EtOAc: Et2O (1:20) and filtered to give 4-[4-amino-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-1-yl]-1-cyclohexanone as a cream solid (3.4 g, 90%), m.pt. 203-205° C.1H NMR (400 MHz, d6-DMSO) 8.28 (1H, s), 7.66 (2H, m), 7.44 (2H, m), 7.08-7.20 (5H, m), 6.1-7.3 (2H, bs), 5.26 (1H, m), 2.71 (2H, m), 2.41 (4H, m), 2.24 (2H, m) HPLC: Tr=15.43 mins, 95%.

1. customEvaporate the acetone
2. extractionExtract with EtOAc (3×200 mL)
3. customDry
4. filtrationfilter
5. customevaporate
6. customto leave a solid which
7. customwas triturated with EtOAc: Et2O (1:20)
8. filtrationfiltered