反应详情

温度

60 °C

A mixture of 7-(3-cyclohexyl-3-oxopropyl)-6-(7-hydroxyheptyl)-1,4-dioxaspiro[4,4]nonane (0.5 g.) in hydrochloric acid (20 ml; 1 N) was stirred at 60° C. for 2 hours, cooled to ambient temperature and extracted with diethyl ether. The ethereal extract was washed with water, then dried over sodium sulphate. Removal of the solvent under reduced pressure gave a crude product (0.4 g.) which was purified by preparative thin layer chromatography on silica gel, using a mixture of diethyl ether, ethyl acetate and hexane (2:1:1 v/v) as eluant, to give 7-[2-(3-cyclohexyl-3-oxopropyl)-5-oxocyclopentyl]heptan-1-ol (0.16 g.), νmax 3450 cm-1, 1730 cm-1, 1700 cm-1, 1060 cm-1 ; Elemental analysis: Found: C, 74.6; H, 10.7%; C21H36O3 requires C, 74.95; H, 10.78%.

1. temperaturecooled to ambient temperature
2. extractionextracted with diethyl ether
3. extractionThe ethereal extract
4. washwas washed with water
5. dry with materialdried over sodium sulphate
6. customRemoval of the solvent under reduced pressure
7. customgave a crude product (0.4 g.) which
8. customwas purified by preparative thin layer chromatography on silica gel
9. additiona mixture of diethyl ether, ethyl acetate and hexane (2:1:1 v/v) as eluant