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
PROCEDURE
实验过程
After dissolving 517 mg of (1-benzylpiperidin-4-yl)-(1,3-dihydroisobenzofuran-1-yl)methanone in 5 ml of 1,2-dichloroethane, 0.49 ml of 1-chloroethyl chloroformate was added and the mixture was heated to reflux for 1 hour. The reaction solution was distilled off under reduced pressure, 5 ml of methanol was added to the residue and heating to reflux was continued for 1 hour. The reaction solution was distilled off under reduced pressure, saturated aqueous sodium bicarbonate solution was added and extraction was performed with ethyl acetate. The extract was dried over anhydrous magnesium sulfate and then the solvent was distilled off under reduced pressure to obtain 104 mg of (1,3-dihydroisobenzofuran-1-yl)-(piperidin-4-yl)methanone hydrochloride.
WORKUP
后处理
- additionwas added
- temperaturethe mixture was heated
- temperatureto reflux for 1 hour
- distillationThe reaction solution was distilled off under reduced pressure, 5 ml of methanol
- additionwas added to the residue
- temperatureheating
- temperatureto reflux
- distillationThe reaction solution was distilled off under reduced pressure, saturated aqueous sodium bicarbonate solution
- additionwas added
- extractionextraction
- dry with materialThe extract was dried over anhydrous magnesium sulfate
- distillationthe solvent was distilled off under reduced pressure