反应详情

A mixture of 50 g of 3-methoxy-4-hydroxybenzeneacetic acid ethyl ester, 66.1 g of powdered potassium carbonate, 70.57 g of 1-bromotetradecane and 500 ml of acetone is heated at reflux temperature for 76 hours. The reaction is cooled, filtered and the filtrate concentrated in vacuo. The residue is dissolved in methylene chloride, washed with 2% sodium bicarbonate and saturated sodium chloride, dried and concentrated in vacuo. The residue is purified by column chromatography (silica gel:0-10% ethyl acetate/hexane) to give 66.6 g of the desired product as colorless crystals.

1. temperatureis heated
2. temperatureat reflux temperature for 76 hours
3. temperatureThe reaction is cooled
4. filtrationfiltered
5. concentrationthe filtrate concentrated in vacuo
6. dissolutionThe residue is dissolved in methylene chloride
7. washwashed with 2% sodium bicarbonate and saturated sodium chloride
8. customdried
9. concentrationconcentrated in vacuo
10. customThe residue is purified by column chromatography (silica gel:0-10% ethyl acetate/hexane)