反应详情

To a solution of diethyl[2-bromo-5-(trifluoromethyl)benzyl]malonate (22.9 g, 57.6 mmol) in ethanol (100 mL) and water (50 mL) was added a 5 M solution of sodium hydroxide in water (30 mL). The mixture was heated to reflux for 2 h. Ethanol was removed by evaporation. The aqueous layer was extracted with ether and then acidified with concentrated HCl to pH 5 at which time a lot of white solid precipitated out. The solid was collected by filtration. The filtrate was extracted with ethyl acetate twice, and the extracts were washed with brine, dried (MgSO4) and concentrated to give a white solid.

1. temperatureThe mixture was heated
2. temperatureto reflux for 2 h
3. customEthanol was removed by evaporation
4. extractionThe aqueous layer was extracted with ether
5. customprecipitated out
6. filtrationThe solid was collected by filtration
7. extractionThe filtrate was extracted with ethyl acetate twice
8. washthe extracts were washed with brine
9. dry with materialdried (MgSO4)
10. concentrationconcentrated
11. customto give a white solid