反应详情

In five equal portions 21 g (200 mmole) of formamidine acetate and 32.5 ml (135 mmole) of a 4.12 M methanol solution of sodium methoxide was added over 3 hr to a solution of 7.2 g (20 mmole) of 8-chloro-1-(2-chlorophenyl)-3,4-dihydro-[(dimethylamino)methylene]-5H-2-benzazepin-5-one in 270 ml of methanol and 270 ml of methylene chloride. The solution was diluted with water and extracted with methylene chloride. The methylene chloride solution was washed with water, dried over anhydrous sodium sulfate, and concentrated at reduced pressure to give an amber oil. Purification by column chromatography (100 g silica gel; eluent 1:1 methylene chloride and ethyl acetate) gave end poduct mp 122°-124° C. Recrystallization from ether gave pale yellow prisms, mp 122°-125° C.

1. extractionextracted with methylene chloride
2. washThe methylene chloride solution was washed with water
3. dry with materialdried over anhydrous sodium sulfate
4. concentrationconcentrated at reduced pressure
5. customto give an amber oil
6. customPurification by column chromatography (100 g silica gel; eluent 1:1 methylene chloride and ethyl acetate)
7. customgave end
8. customRecrystallization from ether
9. customgave pale yellow prisms, mp 122°-125° C.