反应详情

温度

0 °C

Dissolve 3-(2,6-Dichloro-4-methoxybenzyl)-1-(4-oxocyclohexyl)-pyrrolidin-2-one (Preparation 17) (2.09 g, 5.4 mmol) in dichloromethane (50 mL) and ethanol (0.06 mL, 1.08 mmol) and cool to 0° C. Add deoxo-fluor (1.69 mL, 9.18 mmol) over several minutes. Stir overnight at room temperature. Add saturated sodium bicarbonate and extract aqueous layer with dichloromethane. Wash the organic layer with brine and dry with Na2SO4, filter and concentrate to dryness. Purify the crude mixture over silica gel (4/1 hexane in ethyl acetate) to give 650 mg (32%) of the title compound: mass spectrum (m/e): 374 (M+1).

1. extractionAdd saturated sodium bicarbonate and extract aqueous layer with dichloromethane
2. washWash the organic layer with brine
3. dry with materialdry with Na2SO4
4. filtrationfilter
5. concentrationconcentrate to dryness
6. customPurify the crude mixture over silica gel (4/1 hexane in ethyl acetate)