反应详情

5-Amino-2-(N,N-dimethylamino)-pyridine-4-carboxylic acid (0.54 g) was treated with formamidine acetate (3.12 g) in glacial acetic acid (20 ml) and heated at reflux for 16 hours. The mixture was cooled, evaporated to dryness in vacuo and partitioned between ethyl acetate and water. The organic phase was separated, dried over magnesium sulphate and concentrated in vacuo to give, after chromatography on silica, the title compound (0.25 g); δH CDCl3 9.10(1H,d), 8.80(1H,s), 8.31(1H,s), 7.07(1H,s), 3.20(6H,s); m/z (M+1+)191.

1. temperatureheated
2. temperatureat reflux for 16 hours
3. temperatureThe mixture was cooled
4. customevaporated to dryness in vacuo
5. custompartitioned between ethyl acetate and water
6. customThe organic phase was separated
7. dry with materialdried over magnesium sulphate
8. concentrationconcentrated in vacuo
9. customto give