反应详情

A mixture of 2.8 g (7.8 mmole) of 8-chloro-1-(2-chlorophenyl)-3,4-dihydro-4-[(dimethylamino)methylene]-5H-2-benzazepin-5-one, 2.8 g (37 mmole) of thiourea, and 8.0 ml (32 mmole) of a 4.0M methanol solution of sodium methoxide in 80 ml of methanol was stirred at room temperature for 18 hr. The mixture was diluted with water and extracted with ether. The aqueous layer was neutralized with acetic acid and extracted with methylene chloride. The methylene chloride solution was dried over anhydrous sodium sulfate and concentrated at reduced pressure to give a yellow solid, mp 238°-239° C. Recrystallization from tetrahydrofuran gave yellow crystals, mp 232°-234° C.

1. extractionextracted with ether
2. extractionextracted with methylene chloride
3. dry with materialThe methylene chloride solution was dried over anhydrous sodium sulfate
4. concentrationconcentrated at reduced pressure
5. customto give a yellow solid, mp 238°-239° C
6. customRecrystallization from tetrahydrofuran
7. customgave yellow crystals, mp 232°-234° C.