反应详情

Heat 3-benzyloxy-5-fluoro-benzaldehyde (3.75 g, 16.29 mmol), nitromethane (4.08 g, 66.79 mmol), and ammonium acetate (3.47 g, 44.96 mmol) in acetic acid (54 mL) in 125° C. oil bath under nitrogen for 4 hours. Cool to room temperature and pour into ice/water. Extract with hexanes/ethyl acetate. Dry (magnesium sulfate), filter and concentrate. Purify on 120 g silica gel eluting with 100:0 to 80:20 hexanes:ethyl acetate to give 3.05 g (68.5%) of the desired compound as a yellow oil.

1. extractionExtract with hexanes/ethyl acetate
2. dry with materialDry (magnesium sulfate)
3. filtrationfilter
4. concentrationconcentrate
5. customPurify on 120 g silica gel eluting with 100:0 to 80:20 hexanes