反应详情

A mixture of 15.55 g of 4-[(2-ethyl-4-tetradecylphenoxy)methyl]-2,2-dimethyl-1,3-dioxolane, 10 ml of 5% hydrochloric acid and 300 ml of tetrahydrofuran was heated at reflux for 4 hours, then cooled and 1/2 of the solvent evaporated at reduced pressure. The remainder was diluted with ethyl acetate, washed with aqueous sodium bicarbonate, dried and the solvents evaporated. The residue was chromatographed on silica gel, eluting first with hexane:ethyl acetate (8:1), then (4:1), giving 12.1 g of the desired compound, mp 55°-56° C.

1. temperaturewas heated
2. temperatureat reflux for 4 hours
3. temperaturecooled
4. custom1/2 of the solvent evaporated at reduced pressure
5. additionThe remainder was diluted with ethyl acetate
6. washwashed with aqueous sodium bicarbonate
7. customdried
8. customthe solvents evaporated
9. customThe residue was chromatographed on silica gel
10. washeluting first with hexane:ethyl acetate (8:1)