反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To 213 mg of 4-({[3-({(tert-butoxycarbonyl)[(1R)-1-(1-naphthyl)ethyl]amino}methyl)-4-(2-fluorophenyl)piperidin-1-yl]carbonyl}oxy)benzoic acid was added 3.0 mL of a 4 M hydrogen chloride/1,4-dioxane solution, followed by stirring at room temperature overnight. The reaction mixture was concentrated under reduced pressure, and to the obtained residue was added chloroform, followed by washing with a saturated aqueous sodium hydrogen carbonate solution (1.0 mL). The organic layer was dried over anhydrous sodium sulfate, and then filtered, and the filtrate was concentrated under reduced pressure. The obtained residue was dissolved in ethyl acetate, and hexane was added thereto. Then, the precipitate was isolated by filtration. It was dried under reduced pressure to obtain 135 mg of 4-({[4-(2-fluorophenyl)-3-({[(1R)-1-(1-naphthyl)ethyl]amino}methyl)piperidin-1-yl]carbonyl}oxy)benzoic acid as a white solid.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under reduced pressure
- additionto the obtained residue was added chloroform
- washby washing with a saturated aqueous sodium hydrogen carbonate solution (1.0 mL)
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationthe filtrate was concentrated under reduced pressure
- dissolutionThe obtained residue was dissolved in ethyl acetate
- additionhexane was added
- customThen, the precipitate was isolated by filtration
- customIt was dried under reduced pressure