反应详情

A mixture of 1 g (2.8 mmole) of 8-chloro-1-(2-chlorophenyl)-4-[(dimethylamino)methylene]-3,4-dihydro-5H-2-benzazepine-5-one-2-oxide, 1.0 g (11 mmole) of acetamidine hydrochloride and 2.0 ml (9.9 mmole) of a 4.46M methanol solution of sodium methoxide in a mixture of 20 ml of methanol and 20 ml of methylene chloride was stirred at room temperature for 2 hr. The mixture 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 dryness. Recrystallization of the residue from a mixture of ether and methylene chloride gave a colorless solid, mp 215°-216° 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 to dryness
5. customRecrystallization of the residue
6. additionfrom a mixture of ether and methylene chloride
7. customgave a colorless solid, mp 215°-216° C.