反应详情

A 40% aqueous dimethylamine solution (2000 cc) is added to 4-carboxy-6-chloropyrimidine (93.6 g). The mixture is allowed to stand for 3 days and then concentrated to dryness under reduced pressure. The residue is dissolved in water (300 cc). The solution is made alkaline by the addition of sodium bicarbonate powder to a pH of 8 to 9. The solution is then extracted with diisopropyl ether (1000 cc). The aqueous phase is acidified with 12N hydrochloric acid to a pH of 2 to 3. The precipitate is filtered off, washed with ice-water (30 cc) and then with isopropanol (120 cc). 4-Carboxy-6-dimethylaminopyrimidine (73.6 g), melting at 250° C., is obtained.

1. concentrationconcentrated to dryness under reduced pressure
2. dissolutionThe residue is dissolved in water (300 cc)
3. additionby the addition of sodium bicarbonate powder to a pH of 8 to 9
4. extractionThe solution is then extracted with diisopropyl ether (1000 cc)
5. filtrationThe precipitate is filtered off
6. washwashed with ice-water (30 cc)