反应详情

温度

85 °C

A mixture of compound 2 (11.02 g, 0.042 mol) and trans-1-phenyl-1,3-butadiene (8.0 g, 0.062 mol) in 500 ml of toluene is heated to 85° C. and held there for 72 hours, cooled and evaporated to dryness. The oil that remained is purified by flash chromatography on silica gel (eluent comprised of 98% CHCl3 and 2% MeOH by volume). The resulting semisolid is dissolved in chloroform, decolorized with carbon, and filtered through a bed of celite. The solvent is evaporated and the resulting tan solid recrystallized from ethyl acetate/hexane, m.p. 166°-169° C. (Found: C, 78.68; H, 6.39; N, 10.60. C26H25N3O requires: C, 78.96; H, 6.37; N, 10.62).

1. temperaturecooled
2. customevaporated to dryness
3. customThe oil that remained is purified by flash chromatography on silica gel (eluent comprised of 98% CHCl3 and 2% MeOH by volume)
4. dissolutionThe resulting semisolid is dissolved in chloroform
5. filtrationfiltered through a bed of celite
6. customThe solvent is evaporated
7. customthe resulting tan solid recrystallized from ethyl acetate/hexane, m.p. 166°-169° C. (Found: C, 78.68; H, 6.39; N, 10.60. C26H25N3O requires: C, 78.96; H, 6.37; N, 10.62)