反应详情

A solution of 4-cyano-4-[3-cyclopentyloxy-4-(4-fluorobenzyloxy)phenyl)cyclohexan-1-one (0.525 g, 1.49 mmol) and hydroxylamine hydrochloride (0.114 g, 1.63 mmol) in pyridine (5 mL) was stirred at room temperature under an argon atmosphere for 18 h. The mixture was partitioned between 1 N hydrochloric acid and methylene chloride, the organic extract was dried (magnesium sulfate) and the solvent was removed in vacuo. Purification by flash chromatography, eluting with 35% ethylacetate/hexanes, provided a white solid (0.45 g, 82%): m.p. 55°-57° C.

1. customThe mixture was partitioned between 1 N hydrochloric acid and methylene chloride
2. extractionthe organic extract
3. dry with materialwas dried (magnesium sulfate)
4. customthe solvent was removed in vacuo
5. customPurification by flash chromatography
6. washeluting with 35% ethylacetate/hexanes