反应详情

Methyl 5,6-diaminonicotinate (0.9 g, 5.4 mmol) and 3-bromo-2-butanon (0.9 g, 6.0 mmol) were added to acetonitril (30 ml) and refluxed for 24 h. Upon cooling some of the product was filtered off as hydrobromide salt. 20 ml of the filtrate was evaporated under reduced pressure and diethyl ether was added. More product was filtrated off as hydrobromide salt. The salt was dissolved in methylene chloride and washed with a bicarbonate solution. The organic layer was separated, dried over Na2SO4 and evaporated under reduced pressure to give 0.7 g (59%) of the desired compound.

1. temperaturerefluxed for 24 h
2. temperatureUpon cooling some of the product
3. filtrationwas filtered off as hydrobromide salt
4. custom20 ml of the filtrate was evaporated under reduced pressure and diethyl ether
5. additionwas added
6. filtrationMore product was filtrated off as hydrobromide salt
7. dissolutionThe salt was dissolved in methylene chloride
8. washwashed with a bicarbonate solution
9. customThe organic layer was separated
10. dry with materialdried over Na2SO4
11. customevaporated under reduced pressure