反应详情

温度

60 °C

To a solution of (R)—N-methyl-N-(piperidin-3-yl)-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine (310 mg, 0.85 mmol) in EtOH (7.5 mL) was added conc. HCl (2.5 mL) and the reaction mixture was heated at 60° C. for 5 h. The reaction mixture was concentrated in vacuo and the residue was dissolved in MeOH (5 mL) and treated with a polymer supported carbonate resin. The reaction mixture was filtered and the filtrate was concentrated in vivo to yield the titled intermediate (189 mg, 95%), which was used further without further purification. 1H NMR (400 MHz, CD3OD): δ 8.23 (s, 1H), 8.21 (s, 1H), 3.31 (s, 3H), 3.30 (m, 1H), 3.09 (m, 2H), 2.89 (t, J=11.2 Hz, 1H), 2.63 (dt, J=2.8, 12.8 Hz, 1H), 1.93 (m, 2H), 1.76 (m, 2H), 1.75 (m, 1H), 1.35 (m, 1H). LC-MS: m/z [M+1]=233.

1. concentrationThe reaction mixture was concentrated in vacuo
2. dissolutionthe residue was dissolved in MeOH (5 mL)
3. additiontreated with a polymer
4. filtrationThe reaction mixture was filtered
5. concentrationthe filtrate was concentrated in vivo