反应详情

N-Chlorosuccinimide (3.0 g, 22.5 mmol) was added in portions over 1 hour to a stirred solution of 7-chloroquinaldine (3.3 g, 18.5 mmol) and dibenzoyl peroxide (0.1 g) in carbon tetrachloride (100 ml) under reflux. The mixture was heated under reflux for 24 hours adding further N-chlorosuccinimide (0.5 g and 1.0 g) after 3 hours and 20 hours. The mixture was cooled and filtered and the filtrate was extracted with 2M hydrochloric acid (5×40 ml). The extract was basified and re-extracted with dichloromethane and the extract was dried and evaporated to give the product contaminated with 7-chloroqinaldine.

1. temperatureunder reflux
2. temperatureThe mixture was heated
3. temperatureunder reflux for 24 hours
4. custom20 hours
5. temperatureThe mixture was cooled
6. filtrationfiltered
7. extractionthe filtrate was extracted with 2M hydrochloric acid (5×40 ml)
8. extractionre-extracted with dichloromethane
9. customthe extract was dried
10. customevaporated
11. customto give the product