反应详情

To a 500 mL round bottom flask was added 3-methoxy-N-phenylbenzimidamide (7.81 g, 34.5 mmol), 2-chloroacetaldehyde solution (50%, 9.4 mL, 69 mmol), sodium bicarbonate (5.80 g, 69 mmol), and 150 mL 2-propanol. The reaction mixture was heated at reflux for 3 h under nitrogen. The solvent was removed under vacuum and the residue dissolved in ethyl acetate. The ethyl acetate solution was washed with water, brine, dried over magnesium sulfate, filtered, and evaporated. The residue was purified by column chromatography eluting with 50% and 100% ethyl acetate/hexane to give pure product (6.52 g, 75%).

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 3 h under nitrogen
3. customThe solvent was removed under vacuum
4. dissolutionthe residue dissolved in ethyl acetate
5. washThe ethyl acetate solution was washed with water, brine
6. dry with materialdried over magnesium sulfate
7. filtrationfiltered
8. customevaporated
9. customThe residue was purified by column chromatography
10. washeluting with 50% and 100% ethyl acetate/hexane