反应详情

温度

150 °C

A solution of potassium hydroxide (0.2 g) in water (10 ml) was added to a solution of 1-cyano-1,1-diphenyl-3-[N-methyl-N-(3-phenylprop-1-yl)amino]propane (0.22 g-see Preparation 23) in ethanol (10 ml) and the mixture was heated at 150° C. for 20 hours in a stainless steel pressure vessel then concentrated in vacuo. Water (30 ml) was added to the residue and the mixture was extracted with dichloromethane (3×30 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 dichloromethane containing methanol (0% up to 10%). The product-containing fractions were combined and concentrated in vacuo to give the title compound as a viscous gum, yield, 0.11 g.

1. concentrationthen concentrated in vacuo
2. additionWater (30 ml) was added to the residue
3. extractionthe mixture was extracted with dichloromethane (3×30 ml)
4. dry with materialThe combined dichloromethane extracts were dried (Na2SO4)
5. concentrationconcentrated in vacuo
6. customto give a gum which
7. customwas purified by column chromatography on silica eluting with dichloromethane
8. additioncontaining methanol (0% up to 10%)
9. concentrationconcentrated in vacuo