HRID19533
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
3-Oxo-3-m-tolylpropionic acid-ethyl ester (1 g, 4.84 mmol) obtained in Step 1 was dissolved in benzene, and benzaldehyde, acetic acid (0.15 g, 2.49 mmol) and piperidine (0.06 g, 0.8 mmol) were added thereto, followed by refluxing for 4 hrs. Upon the completion of the reaction, the mixture washed successively with saturated saline and saturated sodium bicarbonate, and extracted with ethyl acetate. The organic layer was separated, dried over anhydrous MgSO4 and concentrated under a reduced pressure. The resulting residue was purified by flash chromatography to obtain 1 g of the titled compound (yield: 70%).
WORKUP
后处理
- temperatureby refluxing for 4 hrs
- customUpon the completion of the reaction
- washthe mixture washed successively with saturated saline and saturated sodium bicarbonate
- extractionextracted with ethyl acetate
- customThe organic layer was separated
- dry with materialdried over anhydrous MgSO4
- concentrationconcentrated under a reduced pressure
- customThe resulting residue was purified by flash chromatography