反应详情

The ketone of Example 6 (1 g), ethanol (20 ml) hydroxylamine hydrochloride (280 mg) and potassium carbonate (330 mg) were refluxed together for 2 hours. Thin layer chromatography, using 15% acetone in petrol as eluant, showed partial conversion. Additional quantities of hydroxylamine hydrochloride (280 mg) and potassium carbonate (330 mg) were added three times, with refluxing for 2 hours after each addition. Water was then added, and the mixture was extracted with diethyl ether. The ether extract was dried over magnesium sulphate and evaporated and the residue was purified on a silica gel column using 5% acetone in petrol as eluant to give 1 g (94%) of the desired product.

1. temperaturewith refluxing for 2 hours
2. additionafter each addition
3. extractionthe mixture was extracted with diethyl ether
4. extractionThe ether extract
5. dry with materialwas dried over magnesium sulphate
6. customevaporated
7. customthe residue was purified on a silica gel column