反应详情

温度

5 °C

3 g (18 mmol) of (3-hydroxyphenoxy)acetone and 400 ml of a 0.1M potassium hydroxide solution are introduced into a 1 l three-necked flask equipped with a reflux condenser. Heating is carried out at reflux for 6 hours. The reaction mixture is cooled to 5° C., a molar hydrochloric acid solution is added, in order to obtain a pH of approximately 5, and extraction is carried out with ethyl ether (3×150 ml). The organic phases are combined, dried over magnesium sulphate and concentrated. The residue is purified by silica column chromatography (elution solvent: 8/2 cyclohexane/ethyl acetate). 1.61 g of 3-methyl-6-hydroxybenzofuran are obtained--M.p.: 92° C.

1. customequipped with a reflux condenser
2. temperatureHeating
3. temperatureat reflux for 6 hours
4. customto obtain
5. extractiona pH of approximately 5, and extraction
6. dry with materialdried over magnesium sulphate
7. concentrationconcentrated
8. customThe residue is purified by silica column chromatography (elution solvent: 8/2 cyclohexane/ethyl acetate)