反应详情

3.3 g (0.014 mole) of 6-(2,3-epoxypropoxy)-2,3,4,5-tetrahydro-1H-1-benzazepin-2-one are dissolved in 400 ml of n-propanol, 3 g of isopropylamine are added and the mixture is kept on a boiling waterbath for from 4 to 6 hours. The solvent and excess amine are then distilled off on a rotary evaporator and the residue is twice taken up in methanol, the solvent again being distilled off. The residue thus obtained is chromatographed on a silica gel column, using methanol as the mobile phase. 1.65 g (39.9% yield) of 6-(2-hydroxy-3-isopropylaminopropoxy)-2,3,4,5-tetrahydro-1H-1-benzazepin-2-one, of melting point 143°-145° C., are obtained.

1. customis kept on a boiling waterbath for from 4 to 6 hours
2. distillationThe solvent and excess amine are then distilled off on a rotary evaporator
3. distillationthe solvent again being distilled off
4. customThe residue thus obtained
5. customis chromatographed on a silica gel column