反应详情

温度

60 °C

80 g of the product which was obtained above were suspended in 140 ml of dimethylformamide. A solution of 72.6 g of potassium phthalimide in 205 ml of dimethylformamide was added to the suspension and the mixture was then stirred at 60° C. for 16 hours. For the working-up, it was cooled down to room temperature and 800 ml of water were slowly added dropwise; the mixture was then stirred for 2 hours while cooling with ice. The resulting crystal slurry was filtered out with suction, washed firstly with a water/dimethylformamide mixture and then with methyl tert-butyl ether, and subsequently dried at 60° C. for 2 days under reduced pressure. 73.3 g of 4,5-dihydro-3-phthalimido-1H-1-benzazepin-2 (3H) -one were obtained with a melting range of from 185° to 195° C.

1. temperatureit was cooled down to room temperature
2. stirringthe mixture was then stirred for 2 hours
3. temperaturewhile cooling with ice
4. filtrationThe resulting crystal slurry was filtered out with suction
5. washwashed firstly with a water/dimethylformamide mixture
6. dry with materialwith methyl tert-butyl ether, and subsequently dried at 60° C. for 2 days under reduced pressure