反应详情

In 1,2-dimethoxyethane (10 ml) was suspended 60% sodium hydride (dispersion in paraffin) (132 mg). To the suspension was added dropwise, while stirring, a solution of diethylphosphonoacetic acid morpholide (688 mg) in 1,2-dimethoxyethane (5 ml). To the mixture was added 2-(2-chlorophenoxy)-5-(3,4-dimethoxybenzoyl)pyridine (800 mg), which was heated for 8 hours under reflux. The reaction mixture was concentrated and the residue was dissolved in ether, washed with water and dried over anhydrous magnesium sulfate. The solvent was then distilled off to leave an oily substance, which was purified by means of a silica gel chromatography (eluted with ethyl acetate) to obtain 4-[3-(2-(2-chlorophenoxy)-5-pyridyl)-3-(3,4-dimethoxyphenyl)acryloyl]morpholine (Compound No.1) (330 mg) as a resinous solid.

1. additionTo the suspension was added dropwise
2. temperaturewas heated for 8 hours
3. temperatureunder reflux
4. concentrationThe reaction mixture was concentrated
5. dissolutionthe residue was dissolved in ether
6. washwashed with water
7. dry with materialdried over anhydrous magnesium sulfate
8. distillationThe solvent was then distilled off
9. customto leave an oily substance, which
10. customwas purified by means of a silica gel chromatography (eluted with ethyl acetate)