反应详情

A mixture of 3.5 g (10 mmole) of 1-(2-chlorophenyl)-3,4-dihydro-4-[(dimethylamino)methylene]-5H-2-benzazepin-5-one, 4.8 g (40 mmole) of isobutyramidine hydrochloride, 10 ml (41 mmole) of a 4.12M methanol solution of sodium methoxide and 100 ml of methanol was stirred at room temperature for 2 hr. 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 ether gave a light yellow solid, mp 127°-129° C. Recrystallization from a mixture of ether and petroleum ether gave colorless rods, mp 127°-129° 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 ether
6. customgave a light yellow solid, mp 127°-129° C
7. customRecrystallization
8. additionfrom a mixture of ether and petroleum ether
9. customgave colorless rods, mp 127°-129° C.