Potassium Carbonate → 1H-1-Benzazepine
反応式
CO[C:3]1[C:18](OC)=[CH:17][C:6]2[CH2:7][C:8](=O)[N:9](CCCI)[CH:10]=[CH:11][C:5]=2[CH:4]=1.C(=O)([O-])[O-].[K+].[K+]>O>[NH:9]1[C:10]2[CH:11]=[CH:5][CH:4]=[CH:3][C:18]=2[CH:17]=[CH:6][CH:7]=[CH:8]1参加物
4
反応条件
- 温度
- 52.5 °C
実験手順
7,8-Dimethoxy-3-[3-iodopropyl]-1,3-dihydro-2H-3-benzazepin-2-one (38 g) and potassium carbonate (60 g) were added to a mixture of (S)—N-[(4,5-dimethoxybenzocyclobut-1-yl)-methyl]-N-(methyl)amine (20 g) and demineralized water (100 ml) at room temperature. The reaction mixture was heated and stirred at 50-55° C. for 12-16 hours. After completion of reaction, reaction mass was cooled to 25-30° C. and the product is extracted in ethyl acetate (100 ml). The aqueous layer was further extracted with ethyl acetate (60 ml). Combined ethyl acetate layers was acidified with aqueous hydrochloric acid and stirred. The layers were separated and pH of the aqueous layer was adjusted to 10.5-12.5 with aqueous sodium hydroxide solution. The aqueous layer is extracted with ethyl acetate (140 ml+60 ml). Ethyl acetate was distilled out completely under vacuum to get the title compound.