反应详情

1-(2-hydroxyethyl)-6-hydroxy-2,3,4,5-tetrahydro-1H-1-benzazepine (52 mg) was dissolved in DMF (3 ml), and the resultant solution was stirred at room temperature. Potassium carbonate (122 mg) and methyl bromoacetate (0.035 ml) were added to the solution, and the mixture was stirred at room temperature. After disappearance of the raw materials was confirmed, water (20 ml) was added to the reaction solution, and the mixture was then extracted with ethyl acetate. The resultant organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and then concentrated. The resultant residue was purified by column chromatography (silica gel:hexane/ethyl acetate=2/1) to obtain the object compound (47 mg, yield 67%).

1. extractionthe mixture was then extracted with ethyl acetate
2. washThe resultant organic layer was washed with saturated brine
3. dry with materialdried over anhydrous sodium sulfate
4. concentrationconcentrated
5. customThe resultant residue was purified by column chromatography (silica gel:hexane/ethyl acetate=2/1)