反应详情

4N HCl in dioxane (5 mL) was added to (S)-tert-butyl 2-((S)-1-(4-chlorophenyl)-2-(4-(5-methyl-1H-pyrazolo[3,4-b]pyridin-4-yl)piperazin-1-yl)-2-oxoethyl)pyrrolidine-1-carboxylate (68 mg, 0.13 mmol), and the mixture was stirred at room temperature. After 30 minutes, the solvent was removed under reduced pressure, and the resulting residue was triturated with ether. The solid material was filtered, washed with additional ether (2×2 mL) and dried under high vacuum for 24 hours to provide (S)-2-(4-chlorophenyl)-1-(4-(5-methyl-1H-pyrazolo[3,4-b]pyridin-4-yl)piperazin-1-yl)-2-((S)-pyrrolidin-2-yl)ethanone dihydrochloride (62 mg, 0.12 mmol, 96% yield) as a solid. LCMS (APCI+) m/z 439.1 (M+H)+. NMR (400 Hz, DMSO-d6) δ 9.98 (brs, 1H), 9.06 (s, 1H), 8.23 (s, 1H), 7.49 (d, 2H), 7.43 (d, 2H), 4.56 (d, 1H), 4.03-3.96 (m, 2H), 3.93-3.87 (m, 3H), 3.71-3.65 (m, 1H), 3.64-3.57 (m, 2H), 3.50-3.46 (m, 1H), 3.19-3.13 (m, 2H), 2.31 (s, 3H), 1.97-1.89 (m, 1H), 1.78-1.70 (m, 1H), 1.63-1.52 (m, 2H).

1. customthe solvent was removed under reduced pressure
2. customthe resulting residue was triturated with ether
3. filtrationThe solid material was filtered
4. washwashed with additional ether (2×2 mL)
5. customdried under high vacuum for 24 hours