反应 #46162

反应方程式

3-(3-Benzyloxyphenyl)-3-oxopropionate ethyl ester

isopropylamine

→

2-(3-benzyloxybenzoyl)-N-isopropyl-3-phenylacryl amide

收率 108.9%

溶剂

m-xylene

反应条件

后处理

1. 1
   温度the reaction mixture was refluxed
2. 2
   workup.STIRRINGAfter stirring
3. 3
   温度refluxing for 24 hours at room temperature
4. 4
   萃取the organic layer was extracted with saturated sodium chloride and ethyl acetate
5. 5
   干燥dried over anhydrous magnesium sulfate
6. 6
   浓缩concentrated
7. 7
   其他resulting residue
8. 8
   其他was purified by column chromatography (ethyl acetate:hexane=1:2)

实验过程

3-(3-Benzyloxyphenyl)-3-oxopropionate ethyl ester (174.42 g, 584.47 mmol) was dissolved in m-xylene and the reaction mixture was refluxed while stirring for 30 min at 150° C. Then, isopropylamine (38 g, 642.92 mmol) was added dropwise to the mixture. After stirring and refluxing for 24 hours at room temperature, the organic layer was extracted with saturated sodium chloride and ethyl acetate, dried over anhydrous magnesium sulfate, concentrated, and resulting residue was purified by column chromatography (ethyl acetate:hexane=1:2) to obtain 2-(3-benzyloxybenzoyl)-N-isopropyl-3-phenylacryl amide (127.13 g, yield 70%) as yellow oil.

来源