反应详情

A mixture of 36.7 g (0.2 mol) of 6-chloropyridine-2,3-dicarboxylic anhydride, 17.4 g (0.3 mol) of potassium fluoride and 1 g of 18-crown-6 in 200 ml of propionitrile were stirred for 10 hours while refluxing. After cooling, the reaction mixture was filtered with suction and the residue was washed with methylene chloride. The filtrate was evaporated down under reduced pressure and stirred with a 2:1 methyl tert-butyl ether/pentane mixture, and the product was filtered off with suction and dried. 25.3 g (76% of theory) of the title compound of melting point 106° C. (decomposition) were obtained.

1. temperaturewhile refluxing
2. temperatureAfter cooling
3. filtrationthe reaction mixture was filtered with suction
4. washthe residue was washed with methylene chloride
5. customThe filtrate was evaporated down under reduced pressure
6. stirringstirred with a 2:1 methyl tert-butyl ether/pentane mixture
7. filtrationthe product was filtered off with suction
8. customdried