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-Propoxybenzaldehyde (15.47 g) and methyl (triphenylphosphoranylidene)acetate was suspended in toluene (150 ml), and the resulting suspension was heated at reflux for 2 hours. The reaction mixture was diluted with ethyl acetate and was washed respectively with water and an aqueous saturated solution of sodium chloride, and the organic layer was dried with anhydrous magnesium sulfate. After concentration under reduced pressure to remove the solvent, the precipitated triphenylphosphine oxide was removed and was washed with ether. The filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=6:1) to obtain ethyl 2-propoxycinnamate (21.24 g) as a yellow oil.
WORKUP
后处理
- temperaturethe resulting suspension was heated
- temperatureat reflux for 2 hours
- washwas washed respectively with water
- dry with materialan aqueous saturated solution of sodium chloride, and the organic layer was dried with anhydrous magnesium sulfate
- concentrationAfter concentration under reduced pressure
- customto remove the solvent
- customthe precipitated triphenylphosphine oxide was removed
- washwas washed with ether
- concentrationThe filtrate was concentrated under reduced pressure
- customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=6:1)