反应详情

To a solution of 7-[4-(2-butoxyethoxy)phenyl]-1-(2,2,2-trifluoroacetyl)-2,3-dihydro-1-benzazepine-4-carboxylic acid (500 mg), (4-amino-3-ethoxyphenyl)(2-pyridyl)methanol (320 mg) and 1-hydroxybenzotriazole monohydrate (210 mg) in DMF (15 ml) was added catalytic amount of 4-(N,N-dimethylamino)pyridine, and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (263 mg) was added to the mixture and the mixture was stirred overnight under nitrogen atmosphere. Water was added to the mixture and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over magnesium sulfate. The solvent was distilled off under reduced pressure and the obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:3), and was recrystallized from diisopropyl ether-ethyl acetate, to give 7-[4-(2-butoxyethoxy)phenyl]-N-[2-ethoxy-4-[hydroxy(2-pyridyl)methyl]phenyl]-1-(2,2,2-trifluoroacetyl)-2,3-dihydro-1-benzazepine-4-carboxamide (504 mg) as yellow crystals.

1. additionwas added to the mixture
2. extractionthe mixture was extracted with ethyl acetate
3. washThe organic layer was washed with saturated brine
4. dry with materialdried over magnesium sulfate
5. distillationThe solvent was distilled off under reduced pressure
6. customthe obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:3)
7. customwas recrystallized from diisopropyl ether-ethyl acetate