反应详情

温度

80 °C

Ethyl 4-bromo-3-hydroxybenzoate (1.5 g, 6.12 mmol), potassium carbonate (5.07 g, 36.72 mmol) and 1-chloro-2-methylpropan-2-ol (0.75 mL, 7.34 mmol) were placed in 50 mL DMF and the reaction was heated at 80° C. for 18 h. The mixture was cooled and partitioned between EtOAc and water. The organic layer was separated, washed with water, brine, dried (Na2SO4), filtered, and the filtrate was concentrated under vacuum to an oil. Purification by column chromatography on silica gel using EtOAc/hexane (0-50%) gave the product (0.5 g, 26%) as a yellow oil.

1. temperatureThe mixture was cooled
2. custompartitioned between EtOAc and water
3. customThe organic layer was separated
4. washwashed with water, brine
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationthe filtrate was concentrated under vacuum to an oil
8. customPurification by column chromatography on silica gel