反应详情

To a solution of 0.30 g of 4-(4-aminobenzoyl)-5,6,7,8-tetrahydro-4H-thieno[3,2-b]azepine and 0.208 ml of triethylamine in 10 ml of dichloromethane is added, under argon, 0.251 g of 3,4-dichlorobenzoyl chloride. The mixture is stirred overnight and concentrated to dryness under vacuum. The residue is dissolved in ethyl acetate and the solution washed with H2O, 2N citric acid, NaHCO3 solution, brine and dried (Na2SO4). The solvent is removed and the residual yellow solid crystallized from ethyl acetate-hexane to give 0.254 g of crystals, m.p. 154°-160° C.

1. concentrationconcentrated to dryness under vacuum
2. dissolutionThe residue is dissolved in ethyl acetate
3. washthe solution washed with H2O, 2N citric acid, NaHCO3 solution, brine
4. dry with materialdried (Na2SO4)
5. customThe solvent is removed
6. customthe residual yellow solid crystallized from ethyl acetate-hexane