反应详情

温度

100 °C

2,3-Diamino-4,6-dimethylpyridine (25.0 g, 0.182 mol) was suspended in polyphosphoric acid (465 g), and acetic acid (31.3 mL, 0.547 mol) was added to the suspention, followed by stirring at 100° C. for 3 hours. The reaction mixture was moved to ice water and sodium carbonate (345 g) was added in a little portion while stirring. Then, 28% aqueous ammonium solution was added to the residue to control the pH to 9 and the mixture was stirred for 1 hour. Precipitated crystals were collected by filtration, and was washed with water, and the obtained crystals were dried under reduced pressure at 40° C. overnight to obtain Compound P11 (26.2 g, 0.162 mol, 89%).

1. additionwas added in a little portion
2. stirringwhile stirring
3. stirringthe mixture was stirred for 1 hour
4. customPrecipitated crystals
5. filtrationwere collected by filtration
6. washwas washed with water
7. customthe obtained crystals were dried under reduced pressure at 40° C. overnight
8. customto obtain Compound P11 (26.2 g, 0.162 mol, 89%)