HRID1108752
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
3,4-Dimethoxybenzaldehyde (30.1 g) was dissolved in acetone (900 ml), and then piperidine (23.2 ml) and acetic acid (13.4 ml) were added prior to reflux for 4 hours. After distilling off the reaction solvent under reduced pressure, it was dissolved in 600 ml of ethyl acetate and washed with saturated sodium bicarbonate water and saturated saline. After drying with anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure producing yellow crystals which were then washed in isopropyl ether to give 21.0 g of 4-(3,4-dimethoxyphenyl)-3-buten-2-one (56.4%).
WORKUP
后处理
- temperatureto reflux for 4 hours
- distillationAfter distilling off the reaction solvent under reduced pressure, it
- dissolutionwas dissolved in 600 ml of ethyl acetate
- washwashed with saturated sodium bicarbonate water and saturated saline
- dry with materialAfter drying with anhydrous magnesium sulfate
- distillationthe solvent was distilled off under reduced pressure
- customproducing yellow crystals which
- washwere then washed in isopropyl ether