反应详情

Hydroxylamine hydrochloride (71 mg), triethylamine (0.17 ml) and (±)-3-[2,4-bis(methoxymethoxy)phenyl]cyclohexanone (200 mg) were heated under reflux in ethanol (8 ml). After 0.75 hr, the reaction mixture was evaporated in vacuo and the residue was partitioned between ethyl acetate (100 ml) and water (100 ml). The aqueous layer was extracted with ethyl acetate (2×100 ml), and the combined organic extracts were dried over magnesium sulfate and evaporated in vacuo. The crude residue was purified by flash column chromatography (SiO2, ethyl acetate/petrol, 1:1 v/v) to furnish the title compound as a pale yellow oil (197 mg, 94%); m/z (ES+) 310 (M+H)+.

1. customthe reaction mixture was evaporated in vacuo
2. customthe residue was partitioned between ethyl acetate (100 ml) and water (100 ml)
3. extractionThe aqueous layer was extracted with ethyl acetate (2×100 ml)
4. dry with materialthe combined organic extracts were dried over magnesium sulfate
5. customevaporated in vacuo
6. customThe crude residue was purified by flash column chromatography (SiO2, ethyl acetate/petrol, 1:1 v/v)