反应详情

温度

80 °C

5.0 g (42.0 mmol) of 3-hydroxybenzonitrile and 16.25 ml=21.29 g (109 mmol) of ethyl-bromoisobutyrate were dissolved in 70 ml acetonitrile; then, 17.40 g (126 mmol) of potassium carbonate were added and the reaction mixture stirred for 16 hours at 80° C. (reflux). It was then cooled down to ambient temperature and the solvent was evaporated. The residue was partitioned between water and ether and extracted twice with ether; the organic phases were washed with water, dried (MgSO4) and evaporated. The crude product was purified by flash chromatography (SiO2, heptane/AcOEt) to finally give 9.10 g of the title compound as colorless oil.

1. temperature(reflux)
2. temperatureIt was then cooled down to ambient temperature
3. customthe solvent was evaporated
4. customThe residue was partitioned between water and ether
5. extractionextracted twice with ether
6. washthe organic phases were washed with water
7. dry with materialdried (MgSO4)
8. customevaporated
9. customThe crude product was purified by flash chromatography (SiO2, heptane/AcOEt) to finally give 9.10 g of the title compound as colorless oil