反应详情

A mixture of 0.4 g (1.1 mmol) of 8-chloro-1-(2-chlorophenyl)-3,4-dihydro-4-[(dimethylamino)methylene]-5H-2-benzazepin-5-one and 1.0 g (9.6 mmol) of formamidine acetate in 20 ml of formamidine was heated on a steam bath for 7 hr. The mixture was poured over ice and extracted with methylene chloride. The methylene chloride solution was washed with water, dried over anhydrous sodium sulfate and concentrated at reduced pressure. The residue was triturated with ether to give an off-white solid, mp 215°-217° C.

1. temperaturewas heated on a steam bath for 7 hr
2. additionThe mixture was poured over ice
3. extractionextracted with methylene chloride
4. washThe methylene chloride solution was washed with water
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated at reduced pressure
7. customThe residue was triturated with ether
8. customto give an off-white solid, mp 215°-217° C.