反应详情

A mixture of 45 g of product from Example 62, 62.2 g of 1-bromotetradecane, 58.9 g of powdered potassium carbonate and 500 ml of acetone is heated at reflux temperature for 51 hours. The cooled solution is filtered and 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:5% ethyl acetate) and recrystallized from hexane to give 76.8 g of the desired product.

1. temperatureis heated
2. temperatureat reflux temperature for 51 hours
3. filtrationThe cooled solution is filtered
4. concentrationconcentrated in vacuo
5. dissolutionThe residue is dissolved in methylene chloride
6. washwashed with 2% sodium bicarbonate and saturated sodium chloride
7. customdried
8. concentrationconcentrated in vacuo
9. customThe residue is purified by column chromatography (silica gel:5% ethyl acetate)
10. customrecrystallized from hexane