反应详情

温度

50 °C

To anhydrous acetic acid (0.84 ml) was added dropwise formic acid (0.4 ml), under ice-cooling, and the mixture was stirred, under nitrogen atmosphere, at 50° C. for 2 hours. To the mixture was added THF (5 ml), and to the mixture was added dropwise, under ice-cooling, a solution of methyl 7-bromo-2,3-dihydro-1H-1-benzazepine-4-carboxylate (1.0 g) in THF (15 ml). The mixture was stirred at room temperature overnight. The solvent was evaporated, and to the residue was added water. The mixture was extracted with ethyl acetate. The organic layer was washed with sodium hydrogen carbonate solution, water and saturated brine and dried with anhydrous magnesium sulfate. The solvent was evaporated to give methyl 7-bromo-1-formyl-2,3-dihydro-1H-1-benzazepine-4-carboxylate (1.07 g) as colorless crystals.

1. temperatureunder ice-cooling
2. additionto the mixture was added dropwise, under ice-
3. temperaturecooling
4. stirringThe mixture was stirred at room temperature overnight
5. customThe solvent was evaporated
6. additionto the residue was added water
7. extractionThe mixture was extracted with ethyl acetate
8. washThe organic layer was washed with sodium hydrogen carbonate solution, water and saturated brine
9. dry with materialdried with anhydrous magnesium sulfate
10. customThe solvent was evaporated