反应详情

(±)-3-(2,4-Dihydroxyphenyl)cyclohexanone (13 mg), hydroxylamine hydrochloride (0.0065 g), and triethylamine (16 μl) were heated at 80° C. in DMF (3 ml). After 3 hr, the reaction mixture was partitioned between ethyl acetate and water. The organic layer was washed with brine, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by flash column chromatography (SiO2, petroleum ether/ethyl acetate 3:2 v/v) to furnish the title compound as a white solid (12 mg, 86%). δH (CD3OD) 1.4-2.0 (6H, overlapping m), 2.10 (0.5H, m), 2.20 (0.5H, m), 2.35 (0.5H, m), 2.46 (0.5H, m), 2.94 (1H, m), 6.22-6.26 (2H, overlapping m), 6.92-6.95 (1H, overlapping m); m/z (ES+) 222 (M+H)−.

1. customthe reaction mixture was partitioned between ethyl acetate and water
2. washThe organic layer was washed with brine
3. dry with materialdried over magnesium sulfate
4. customevaporated in vacuo
5. customThe residue was purified by flash column chromatography (SiO2, petroleum ether/ethyl acetate 3:2 v/v)