反応 #1551069

反応方程式

3-bromo-1-cyano-1,1-diphenyl-propane

1-(N-methylamino)-3-phenylpropane

potassium carbonate

→

title compound

1-cyano-1,1-diphenyl-3-[N-methyl-N(3-phenylprop-1-yl)amino]propane

溶媒

acetonitrile

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度under reflux for 48 hours
3. 3
   濃縮concentrated in vacuo
4. 4
   workup.ADDITIONWater (30 ml) was added to the residue
5. 5
   抽出the mixture was extracted with dichloromethane (3×40 ml)
6. 6
   乾燥The combined dichloromethane extracts were dried (Na2SO4)
7. 7
   濃縮concentrated in vacuo
8. 8
   その他to give a gum which
9. 9
   その他was purified by column chromatography on silica eluting with hexane
10. 10
    workup.ADDITIONcontaining dichloromethane (25% up to 100%)
11. 11
    workup.ADDITIONdichloromethane containing methanol (0% up to 4%)
12. 12
    濃縮concentrated in vacuo

実験手順

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.

出典