反应详情

Trifluoroacetic anhydride (20 mL) was added to 2,4,6-trimethyl-pyridine-1-oxide (2.0 g, 14.6 mmol) at 0° C., then the mixture was stirred at room temperature for 5 h. The mixture was concentrated in vacuo, diluted with water and extracted with ethyl acetate. The organic phase was washed with water, dried over anhydrous sodium sulfate and concentrated to afford a residue which was purified by column chromatography on silica gel (60-120 mesh), eluting with 25% ethyl acetate/hexane, to afford (4,6-dimethyl-pyridin-2-yl)-methanol (1.0 g, 50%)-s a dark brown liquid

1. concentrationThe mixture was concentrated in vacuo
2. additiondiluted with water
3. extractionextracted with ethyl acetate
4. washThe organic phase was washed with water
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated
7. customto afford a residue which
8. customwas purified by column chromatography on silica gel (60-120 mesh)
9. washeluting with 25% ethyl acetate/hexane