反应详情

温度

150 °C

A heavy walled, sealable tube suitable for microwave heating was charged with 3 mL of methanol and 40 mg (1.7 mmol) of sodium. The mixture was stirred until all of the sodium had reacted, then 212 mg (1.00 mmol) of 2-bromo-4,6-diaminonicotinonitrile was added. The tube was sealed, and the mixture was heated with a microwave apparatus at 150° C. for 10 minutes then cooled and concentrated under reduced pressure. The residue was suspended in 10 mL of water, and extracted with ethyl acetate (1×20 mL, then 2×10 mL). The combined ethyl acetate layers were back extracted with brine (1×10 mL), dried over MgSO4, filtered, and concentrated to a solid. This was purified via silica gel chromatography, eluting with 60:40 hexanes:ethyl acetate to provide 114 mg (70%) of a white solid.

1. temperatureA heavy walled, sealable tube suitable for microwave heating
2. customhad reacted
3. customThe tube was sealed
4. temperaturethen cooled
5. concentrationconcentrated under reduced pressure
6. extractionextracted with ethyl acetate (1×20 mL
7. extractionThe combined ethyl acetate layers were back extracted with brine (1×10 mL)
8. dry with materialdried over MgSO4
9. filtrationfiltered
10. concentrationconcentrated to a solid
11. customThis was purified via silica gel chromatography
12. washeluting with 60:40 hexanes