反应详情

4-(3-Cyclopentyloxy-4-methoxyphenyl)-4-(fluoromethyl)cyclohexan-1-one dimethyl ketal (0.35 g, 0.95 mmol) in ethyl acetate (2 mL) was treated with 1N hydrochloric acid (2 mL) and the mixture was stirred vigorously and gently heated for 10 min. The mixture was extracted with ethyl acetate, the organic extract was washed with 5% aqueous sodium carbonate, dried (magnesium sulfate) and the solvent was removed in vacuo. Purification by flash chromatography, eluting with 25% ethyl acetate/hexanes, followed by trituration with ether/hexanes, provided a white solid (0.075 g, 24%): m.p. 72°-74 C. Analysis Calc. for C19H25FO3 : C 71.23, H 7.87; found: C 71.22, H 7.70.

1. temperaturegently heated for 10 min
2. extractionThe mixture was extracted with ethyl acetate
3. extractionthe organic extract
4. washwas washed with 5% aqueous sodium carbonate
5. dry with materialdried (magnesium sulfate)
6. customthe solvent was removed in vacuo
7. customPurification by flash chromatography
8. washeluting with 25% ethyl acetate/hexanes