反应详情

4N HCl in dioxane (2 mL) was added to a solution of (S)-tert-butyl 2-((S)-2-(4-(5-chloro-1H-pyrazolo[3,4-b]pyridin-4-yl)piperazin-1-yl)-1-(4-chlorophenyl)-2-oxoethyl)pyrrolidine-1-carboxylate (90 mg, 0.16 mmol) in CH2Cl2 (1 ml). The mixture was stirred at room temperature for 30 minutes. After 30 minutes, the solvent was removed in vacuo, and the resulting residue was triturated with ether. The solid material was filtered, washed with additional ether (2×2 mL) and dried to provide (S)-1-(4-(5-chloro-1H-pyrazolo[3,4-b]pyridin-4-yl)piperazin-1-yl)-2-(4-chlorophenyl)-2-((S)-pyrrolidin-2-yl)ethanone dihydrochloride (71 mg, 0.13 mmol, 83% yield) as a cream solid. LCMS (APCI+) m/z 459.1, 461.1 [(M+H]+. NMR (400 Hz, DMSO-d6) δ 9.61 (br s, 1H), 9.08 (br s, 1H), 8.30 (s, 1H), 8.19 (s, 1H), 7.49 (d, 2H), 7.44 (d, 2H), 4.53 (d, 1H), 4.03-3.96 (m, 1H), 3.79-3.70 (m, 3H), 3.69-3.57 (m, 3H), 3.51-3.45 (m, 1H), 3.21-3.14 (m, 2H), 3.09-3.00 (m, 1H), 1.97-1.89 (m, 1H), 1.78-1.71 (m, 1H), 1.63-1.52 (m, 2H).

1. waitAfter 30 minutes
2. customthe solvent was removed in vacuo
3. customthe resulting residue was triturated with ether
4. filtrationThe solid material was filtered
5. washwashed with additional ether (2×2 mL)
6. customdried