反应详情

A suspension of the crude 1-chloro-4-methylpentan-3-one (about 60 g), aniline (69.8 g, 0.75 mol) and NaHCO3 (210 g, 2.5 mol) in CH3CN (1000 mL) was heated at reflux overnight. After cooling, the insoluble salt was filtered off and the filtrate was concentrated. The residue was diluted with CH2Cl2, washed with 10% HCl solution (100 mL) and brine, dried over Na2SO4, filtered and concentrated to give the crude 4-methyl-1-(phenylamino)-pentan-3-one.

1. temperaturewas heated
2. temperatureat reflux overnight
3. temperatureAfter cooling
4. filtrationthe insoluble salt was filtered off
5. concentrationthe filtrate was concentrated
6. additionThe residue was diluted with CH2Cl2
7. washwashed with 10% HCl solution (100 mL) and brine
8. dry with materialdried over Na2SO4
9. filtrationfiltered
10. concentrationconcentrated