反应详情

In five equal portions 5.5 g (58 mmole) of acetamidine hydrochloride and 15 ml (62 mmole) of a 4.12M methanol solution of sodium methoxide was added over 3 hr. to solution of 3.5 g (10 mmole) of 8-chloro-1-(2-chlorophenyl)-3,4-dihydro-4-[(dimethylamino)methylene]-5H-2-benzazepin-5-one in 140 ml of methanol and 140 ml of methylene chloride. The mixture was diluted with water and extracted with methylene chloride. The methylene chloride solution was washed with water dried with anhydrous sodium sulfate, and concentrated at reduced pressure to give an amber oil. The amber oil was dissolved in 10 ml (10 mmole) of a 1M methanol solution of methanesulfonic acid and the resulting salt was precipitated by the addition of ether to give yellow prisms, mp 193°-197° C. Recrystallization from a mixture of methanol and ether gave yellow prisms, mp 197°-198° C.

1. extractionextracted with methylene chloride
2. washThe methylene chloride solution was washed with water
3. dry with materialdried with anhydrous sodium sulfate
4. concentrationconcentrated at reduced pressure
5. customto give an amber oil
6. customthe resulting salt was precipitated by the addition of ether
7. customto give yellow prisms, mp 193°-197° C
8. customRecrystallization
9. additionfrom a mixture of methanol and ether
10. customgave yellow prisms, mp 197°-198° C.