反应详情

A mixture containing 3-bromo-1-cyano-1,1-diphenyl-propane (1.5 g--see Preparation 4), 1-(N-methylamino)-3-phenylpropane (0.746 g), anhydrous potassium carbonate (1.38 g) and acetonitrile (50 ml) was heated under reflux for 48 hours and then concentrated in vacuo. Water (30 ml) was added to the residue and the mixture was extracted with dichloromethane (3×40 ml). The combined dichloromethane extracts were dried (Na2SO4) and concentrated in vacuo to give a gum which was purified by column chromatography on silica eluting with hexane containing dichloromethane (25% up to 100%) and then dichloromethane containing methanol (0% up to 4%). The product-containing fractions were combined and concentrated in vacuo to give the title compound as a gum, yield, 0.93 g.

1. temperaturewas heated
2. temperatureunder reflux for 48 hours
3. concentrationconcentrated in vacuo
4. additionWater (30 ml) was added to the residue
5. extractionthe mixture was extracted with dichloromethane (3×40 ml)
6. dry with materialThe combined dichloromethane extracts were dried (Na2SO4)
7. concentrationconcentrated in vacuo
8. customto give a gum which
9. customwas purified by column chromatography on silica eluting with hexane
10. additioncontaining dichloromethane (25% up to 100%)
11. additiondichloromethane containing methanol (0% up to 4%)
12. concentrationconcentrated in vacuo