反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
Cis-tert-butyl N-(4-{4-amino-1-[4-(4-methylpiperazino)cyclohexyl]-1H-pyrazolo[3,4-d]pyrimidin-3-yl}phenyl)carbamate (4.0 g, 0.0079 mol) was triturated in anhydrous dichloromethane (75 mL) and the reaction mixture was cooled to 0° C. Trifluoroacetic acid (10 mL) was added dropwise and the resulting solution was warmed up to ambient temperature and stirred under an atmosphere of nitrogen for 1.5 hours. The solvents were removed under reduced pressure, the residue suspended in water (70 mL) and basified with saturated aqueous sodium bicarbonate solution. It was extracted with dichloromethane (3×150 mL), the combined organic extracts were dried with magnesium sulfate and the solvent was removed under reduced pressure to yield cis-3-(4-aminophenyl)-1-[4-(4-methylpiperazino)cyclohexyl]-1H-pyrazolo[3,4-d]pyrimidin-4-amine (3.0 g, 0.00739 mol) as an off-white solid.
WORKUP
后处理
- temperaturethe resulting solution was warmed up to ambient temperature
- customThe solvents were removed under reduced pressure
- extractionIt was extracted with dichloromethane (3×150 mL)
- dry with materialthe combined organic extracts were dried with magnesium sulfate
- customthe solvent was removed under reduced pressure