Acetic Acid → HCID 178423971, compound

Participants

Reaction Conditions

Reaction Steps

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%).

Provenance & Evidence