反应详情

A solution of N[2-methylamino-2-methylpropyl] benzamide (1 g., 0.0052 mole) in methylethyl ketone (MEK) (25 ml.) was added to a solution of 1-bromo-3-methyl-but-2-ene (0.78 g., 0.0052 mole) in MEK (40 ml.) containing sodium carbonate (0.55 g., 0.0052 mole) and a few crystals of sodium iodide. The mixture was heated under reflux for 30 hrs. The inorganic solids were filtered off and the filtrant concentrated by evaporation under reduced pressure to give a liquid residue. This was loaded onto an alumina column and eluted with ethyl acetate. Fractions (25 mls) were collected and concentrated to give N[2-methyl-2[methyl(3-methyl-2-butenyl)amino]propyl]benzamide (1.2 g.).

1. temperatureThe mixture was heated
2. temperatureunder reflux for 30 hrs
3. filtrationThe inorganic solids were filtered off
4. concentrationthe filtrant concentrated by evaporation under reduced pressure
5. customto give a liquid residue
6. washeluted with ethyl acetate
7. customFractions (25 mls) were collected
8. concentrationconcentrated