反应详情

A mixture of 14.2 g of 4-[(2-ethyl-5-tetradecylphenoxy)methyl]-2,2-dimethyl-1,3-dioxolane, 50 ml of 5% hydrochloric acid and 100 ml of tetrahydrofuran was heated at reflux for 8 hours, then allowed to cool and the tetrahydrofuran removed under reduced pressure. Ethyl acetate was added, the mixture washed with water, dried and the solvents removed. The residue was chromatographed on silica gel, eluting impurites with hexane:ethyl acetate (16:1) and then (4:1) to elute the desired compound, giving 11 g, 55.5°-56.5° C.

1. temperaturewas heated
2. temperatureat reflux for 8 hours
3. temperatureto cool
4. customthe tetrahydrofuran removed under reduced pressure
5. additionEthyl acetate was added
6. washthe mixture washed with water
7. customdried
8. customthe solvents removed
9. customThe residue was chromatographed on silica gel
10. washeluting impurites with hexane:ethyl acetate (16:1)
11. wash(4:1) to elute the desired compound
12. customgiving 11 g, 55.5°-56.5° C.