反应详情

Acetamide oxime (500 mg, 6.75 mol) suspended in THF (50 mL) under nitrogen was heated at 60° C. with NaH (132 mg, 5.5 mmol in oil dispersion) for 1 h. Anhydroecgonine methyl ester (2.76 ml) and 4 A° molecular sieves (2 g) were added and the reaction mixture heated under reflux for 3 h. After cooling, the reaction mixture was filtered and the solvent removed in vacuo. The residue was chromatographed on a silica gel column eluting with CHCl3 --CH3OH (95:5) to give the free base.

1. temperaturethe reaction mixture heated
2. temperatureunder reflux for 3 h
3. temperatureAfter cooling
4. filtrationthe reaction mixture was filtered
5. customthe solvent removed in vacuo
6. customThe residue was chromatographed on a silica gel column
7. washeluting with CHCl3 --CH3OH (95:5)
8. customto give the free base