反应详情

In 20 ml of dimethylformamide was dissolved 5.0 g of 3,5-dichloroaniline. To the solution was added 6.16 g of ethyl 3-bromopropionate, followed by heating under reflux for 6 hours. The reaction mixture was concentrated and the concentrate was extracted with ethyl acetate. The extract was washed with saturated sodium hydrogencarbonate aqueous solution and saturated sodium chloride aqueous solution and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure. The residue was subjected-to silica gel column chromatography (eluent: chloroform:hexane=1:1) to yield 3.98 g of the titled compound as a white crystal.

1. temperatureby heating
2. temperatureunder reflux for 6 hours
3. concentrationThe reaction mixture was concentrated
4. extractionthe concentrate was extracted with ethyl acetate
5. washThe extract was washed with saturated sodium hydrogencarbonate aqueous solution and saturated sodium chloride aqueous solution
6. dry with materialdried over anhydrous magnesium sulfate
7. customThe solvent was removed under reduced pressure