反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
TFA (1 mL) was added to tert-butyl 4-(3-(2-tert-butoxyethoxy)-1-(4-methoxybenzyl)-1H-pyrazolo[3,4-b]pyridin-4-yl)piperazine-1-carboxylate (0.080 g, 0.148 mmol) in DCM (1 mL) and stirred at room temperature for 4 hours. The reaction was then concentrated to dryness and dried under vacuum for 3 hours. TFA (2 mL) was then added, and the mixture was heated at 100° C. in a sealed tube for 18 hours. The reaction was then cooled to room temperature and concentrated to dryness. The resulting residue was dissolved in DCM (2 mL), and HCl in ether (1 mL, 2N) was added. The resulting solid was collected by filtration to give 2-(4-(piperazin-1-yl)-1H-pyrazolo[3,4-b]pyridin-3-yloxy)ethanol dihydrochloride (0.050 g, 100%).
WORKUP
后处理
- concentrationThe reaction was then concentrated to dryness
- customdried under vacuum for 3 hours
- additionTFA (2 mL) was then added
- temperaturethe mixture was heated at 100° C. in a sealed tube for 18 hours
- temperatureThe reaction was then cooled to room temperature
- concentrationconcentrated to dryness
- dissolutionThe resulting residue was dissolved in DCM (2 mL)
- additionHCl in ether (1 mL, 2N) was added
- filtrationThe resulting solid was collected by filtration