反应详情

A mixture of 1-hydroxypropan-2-one (1 g, 13.5 mmol) and O-(tetrahydro-2H-pyran-2-yl)hydroxylamine (1.9 g, 16.2 mmol) in methanol (20 mL) and pyridine (7 mL) was treated with acetic acid (0.23 mL, 4 mmol) and stirred at room temperature for 12 hours. The mixture was then concentrated under reduced pressure. The residue was diluted with saturated sodium bicarbonate and extracted with ethyl acetate. The organic extract was concentrated and purified by chromatography (SiO2, eluted with EtOAc-hexane-2:1) to afford 1.8 g of the title compound. MS (DCI/NH3) m/z 174 (M+H)+.

1. concentrationThe mixture was then concentrated under reduced pressure
2. additionThe residue was diluted with saturated sodium bicarbonate
3. extractionextracted with ethyl acetate
4. extractionThe organic extract
5. concentrationwas concentrated
6. custompurified by chromatography (SiO2, eluted with EtOAc-hexane-2:1)