反应详情

温度

150 °C

To a solution of 52.96 g the crude ethyl 3-(2-bromophenyl)-2-ethoxycarbonyl-3-methylpropionate (168.13 mmole) in dimethylsulfoxide (250 ml) and water (3 ml) was added 14 g of lithium chloride, and the mixture was heated at 150° C. for 2.5 hours. After cooling the mixture, dimethylsulfoxide was removed under reduced pressure, and the residue was diluted with an aqueous sodium chloride solution and extracted with ethyl acetate. The organic phase was washed with an aqueous ammonium chloride solution and dried over magnesium sulfate, and the solvent was removed under reduced pressure. The residual concentrate was further purified by distillation to give 28.04 g of ethyl 3-(2-bromophenyl)-3-methylpropionate (65%).

1. customwas removed under reduced pressure
2. additionthe residue was diluted with an aqueous sodium chloride solution
3. extractionextracted with ethyl acetate
4. washThe organic phase was washed with an aqueous ammonium chloride solution
5. dry with materialdried over magnesium sulfate
6. customthe solvent was removed under reduced pressure
7. concentrationThe residual concentrate
8. distillationwas further purified by distillation