反应详情

Mix 3-bromo-4-hydroxy-benzonitrile (1.520 g, 8.0 mmol), alkyl bromide (1.161 g, 9.6 mmol), potassium carbonate (3.317 g, 24 mmol) and potassium iodide (133 mg, 0.1 mmol) in acetone (80 mL). Heat the mixture to reflux for 12 h. Cool to ambient temperature, add EtOAc, wash the organic layer with water, and extract the aqueous layer twice with EtOAc. Dry the combined organic extracts over Na2SO4, filter and concentrate. Purify by chromatography on silica gel eluting with EtOAc/hexane (1:8) to obtain the desired intermediate.

1. temperatureHeat the mixture
2. temperatureto reflux for 12 h
3. washwash the organic layer with water
4. extractionextract the aqueous layer twice with EtOAc
5. dry with materialDry the combined organic extracts over Na2SO4
6. filtrationfilter
7. concentrationconcentrate
8. customPurify by chromatography on silica gel eluting with EtOAc/hexane (1:8)