反应详情

A mixture of 6,11-dihydro-5H-dibenz[b,e]azepine (0.195 g), 4-[([1,1'-biphenyl]-2-carbonyl)amino]benzoyl chloride (0.41 g) and 0.155 g of N,N-diisopropylethylamine in 12 ml of dichloromethane is stirred at room temperature for 3 hours. The mixture is poured into water and extracted with dichloromethane. The extract is washed with H2O, saturated NaHCO3, H2O, brine and dried (Na2SO4). The solution is filtered through a thin pad of hydrous magnesium silicate and the filter pad washed with dichloromethane. The filtrate is concentrated to dryness to give 0.66 g of a yellow l , solid. Chromatography on thick layer silica gel plates with hexane-ethyl acetate (1.5:1) gives crystals (0.165 g) (from dichloromethane-ethyl acetate), m.p. 224° C.-225° C.

1. extractionextracted with dichloromethane
2. washThe extract is washed with H2O, saturated NaHCO3, H2O, brine
3. dry with materialdried (Na2SO4)
4. filtrationThe solution is filtered through a thin pad of hydrous magnesium silicate
5. washthe filter pad washed with dichloromethane
6. concentrationThe filtrate is concentrated to dryness
7. customto give 0.66 g of a yellow l , solid