反应详情

In 10 ml of dimethylformamide was suspended 165 mg of 60% sodium hydride, and 1.0 g of 1-tosyl-2,3,4,5-tetrahydro-1-H-1 -benzazepin-5-one was added to the suspension under ice-cooling, followed by 1 hour of stirring in the ice bath. To this was added dropwise 0.90 ml of dimethyl sulfate, and the mixture was stirred for 30 minutes. After adding ammonium chloride aqueous solution to the reaction solution and subsequently evaporating the solvent, the thus obtained residue was treated with chloroform and water to effect phase separation, and the resulting organic layer was dried over anhydrous magnesium sulfate. The solvent was evaporated and the resulting residue was applied to column chromatography, which was eluted with hexane-ethyl acetate (4:1, v/v) to obtain 621 mg of 5-methoxy-1-tosyl-2,3-dihydro-1H-1-benzazepine.

1. additionwas added to the suspension under ice-
2. temperaturecooling
3. customsubsequently evaporating the solvent
4. additionthe thus obtained residue was treated with chloroform and water
5. customphase separation
6. dry with materialthe resulting organic layer was dried over anhydrous magnesium sulfate
7. customThe solvent was evaporated
8. washwas eluted with hexane-ethyl acetate (4:1