反应详情

温度

78 °C

To a solution of methyl 7-bromo-2,3-dihydro-1-benzazepine-4-carboxylate (200 mg) and pyridine (123 mg) in tetrahydrofuran (10 ml) was added 2-thienyl chloride (208 mg) at 0° C., and the mixture was heated at 78° C. overnight. After allowing to cool, to the mixture was added water, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine and dried with magnesium sulfate. The solvent was evaporated, which was recrystallized from hexane-ethyl acetate to give methyl 7-bromo-1-(2-thienylcarbonyl)-2,3-dihydro-1-benzazepine-4-carboxylate (236 mg) as colorless crystals.

1. temperatureto cool, to the mixture
2. extractionthe mixture was extracted with ethyl acetate
3. washThe organic layer was washed with water and saturated brine
4. dry with materialdried with magnesium sulfate
5. customThe solvent was evaporated
6. customwhich was recrystallized from hexane-ethyl acetate