反应详情

7-(2,6-Difluorobenzyl)-4,7-dihydro-5-isobutyryl-3-methyl-4-oxo-2-phenylthieno[2,3-b]pyridine (10 g), N-bromosuccinimide (4.86 g), 2,2′-azobis(2,4-dimethylvaleronitrile (0.56 g) and methyl acetate (100 ml) were mixed and the reaction mixture was heated under reflux for 2 hours. The reaction mixture was allowed to cool with stirring over a period of 2 hours, water (50 ml) was added and then the mixture was stirred with cooling on ice for 1.5 hours. The crystal precipitated was recovered by a filtration, washed with an ice-cooled methyl acetate (30 ml) and water (30 ml), dried in vacuo at 40° C. for 6 hours to obtain the title compound (10.61 g, 87.1%).

1. temperaturethe reaction mixture was heated
2. temperatureunder reflux for 2 hours
3. temperatureto cool
4. stirringthe mixture was stirred
5. temperaturewith cooling on ice for 1.5 hours
6. customThe crystal precipitated
7. filtrationwas recovered by a filtration
8. washwashed with an ice-
9. temperaturecooled methyl acetate (30 ml) and water (30 ml)
10. customdried in vacuo at 40° C. for 6 hours