反应详情

In two equal portions 14.4 g (80 mmole) of guanidine carbonate and 20 ml (82 mmole) of 4.12M methanol solution of sodium methoxide was added over 90 min to a solution of 3.6 g (10 mmole) of 8-chloro-1-(2-chlorophenyl)-3,4-dihydro-4-[(dimethylamino)methylene]-5H-2-benzazepin-5-one in 100 ml of methanol. The mixture was diluted with water and extracted with methylene chloride. The methylene chloride solution was dried over anhydrous sodium sulfate and concentrated at reduced pressure to give a yellow oil. Crystallization of the oil with methylene chloride gave a white solid, mp 240°-241° C. Recrystallization from a mixture of ether and methylene chloride gave colorless needles, mp 240°-241° C.

1. extractionextracted with methylene chloride
2. dry with materialThe methylene chloride solution was dried over anhydrous sodium sulfate
3. concentrationconcentrated at reduced pressure
4. customto give a yellow oil
5. customCrystallization of the oil with methylene chloride
6. customgave a white solid, mp 240°-241° C
7. customRecrystallization
8. additionfrom a mixture of ether and methylene chloride
9. customgave colorless needles, mp 240°-241° C.