HRID1182614
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
5.00 g (38.4 mmol) of acetoacetic acid and 5.40 g (38.4 mmol) of 3-chlorobenzaldehyde were dissolved in 50 ml of 2-propanol. 327 mg (3.84 mmol) of piperidine and 231 mg (3.84 mmol) of acetic acid were added and stirred at room temperature for one day. After the solvent was evaporated, ethyl acetate was added and the reaction mixture was washed with 1 N hydrochloric acid and saturated aqueous sodium hydrogencarbonate solution. The organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by the silica gel chromatography (hexane/ethyl acetate=5/1) to obtain the title compound.
WORKUP
后处理
- customAfter the solvent was evaporated
- additionethyl acetate was added
- washthe reaction mixture was washed with 1 N hydrochloric acid and saturated aqueous sodium hydrogencarbonate solution
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by the silica gel chromatography (hexane/ethyl acetate=5/1)