HRID245748
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
The impure benzyl((trans)-4-(1-bromo-8-methylimidazo[1,5-a]pyrazin-3-yl)cyclohexyl)methyl(methyl)carbamate (0.299 mmol, 141 mg) in 37% hydrochloric acid (20.94 mmol, 1.745 ml) was stirred for 18 hours at room temperature and one hour at 40° C. The reaction mixture was concentrated in vacuo. The residue dissolved in water and washed with diethyl ether twice. The aqueous layer basified with 2 N aqueous sodium hydroxide and extracted with dichloromethane twice. The combined organic extracts were dried (Na2SO4) and concentrated in vacuo to give impure 1-((trans)-4-(1-bromo-8-methylimidazo[1,5-a]pyrazin-3-yl)cyclohexyl)-N-methylmethanamine (91 mg).
WORKUP
后处理
- concentrationThe reaction mixture was concentrated in vacuo
- dissolutionThe residue dissolved in water
- washwashed with diethyl ether twice
- extractionextracted with dichloromethane twice
- dry with materialThe combined organic extracts were dried (Na2SO4)
- concentrationconcentrated in vacuo