反应详情

A mixture of 0.197 g of 6,11-dihydropyrido[2,3-b][1,5]benzodiazepine, 0.444 g of 4-[([1,1'-biphenyl]-2-carbonyl)amino]-2-chlorobenzoyl chloride and 0.155 g of N,N-diisopropylethylamine in 8 ml of dichloromethane is stirred at room temperature for 1.5 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 filtrate concentrated to dryness. The residue is chromatographed on thick layer silica gel plates with hexane-ethyl acetate (1:2) to give 0.160 g of solid, m.p. 147° C.-165° C. Anal Found: C, 72.1; H, 5.1; N, 9.1; Cl, 6.3.

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. concentrationthe filtrate concentrated to dryness
6. customThe residue is chromatographed on thick layer silica gel plates with hexane-ethyl acetate (1:2)