反应详情

A mixture of ethyl 4-chloro-2-(1-bromoethyl)nicotinate (7.45 g) and sodium bicarbonate (4.00 g) in 50 ml of DMSO is heated at 120°, under nitrogen, for 2 hours, after which it is cooled, diluted with water, filtered and extracted with ether. The combined organic layers are washed with water and concentrated. The residue is taken into ethyl acetate, washed with brine, dried, concentrated and purified by flash chromatography to give 4-chloro-7-methylfuro-[3,4-b]-pyridin-5-(7H)-one, which is then reacted with N-bromosuccinimide and 2,2'-azobis(2-methylpropionitrile), as above, to give 7-bromo-4-chloro-7-methylfuro-[3,4-b]-pyridin-5-(7H)-one.

1. temperatureis heated at 120°, under nitrogen, for 2 hours
2. temperatureafter which it is cooled
3. filtrationfiltered
4. extractionextracted with ether
5. washThe combined organic layers are washed with water
6. concentrationconcentrated
7. washwashed with brine
8. customdried
9. concentrationconcentrated
10. custompurified by flash chromatography