反应详情

A mixture of tert-butyl 4-(5-cyclopropyl-3-iodo-1H-pyrazolo[3,4-b]pyridin-4-yl)piperazine-1-carboxylate (200 mg, 0.426 mmol) and 4N HCl in dioxane (4 mL) was stirred at room temperature for 2 hours. The solvent was then removed in vacuo, and the residue was triturated with CH3CN. The solid formed was filtered, washed with Et2O and dried to provide 5-cyclopropyl-3-iodo-4-(piperazin-1-yl)-1H-pyrazolo[3,4-b]pyridine hydrochloride salt (179 mg, 95% yield) as a solid. 1H NMR (400 MHz, d6-DMSO) δ 9.47 (br s, 2H), 8.32 (s, 1H), 3.67-3.62 (m, 4H), 3.42-3.35 (m, 4H), 2.09-2.03 (m, 1H), 1.07-1.01 (m, 2H), 0.80-0.76 (m, 2H); LCMS (APCI+) m/z 370 (M+H)+, Retention time=1.87 minutes.

1. customThe solvent was then removed in vacuo
2. customthe residue was triturated with CH3CN
3. customThe solid formed
4. filtrationwas filtered
5. washwashed with Et2O
6. customdried