Acetic Acid → HCID 178433163, compound

Participants

Reaction Conditions

Reaction Steps

38.25 Parts of 2-dimethylamino-4-hydroxy-6-methyl pyrimidine, 5 parts of zinc acetate and 7 parts of a 50% aqueous paste of 3% palladium on carbon catalyst are stirred in 180 parts of acetic acid and 180 parts of water in a closed container. Hydrogen is then passed into the reactor to a pressure of 1.5 bar. The temperature is raised to 103° C and the hydrogen pressure to 2.3 bar and 50 parts by volume of an 18% solution of formaldehyde in water are added at a uniform rate over 5 hours to the reaction mixture at 103°-110° C under 2 - 2.3 bar hydrogen pressure. After 11/2 hours the reaction mixture is cooled and the palladium on carbon catalyst removed by filtration. The filtrates are distilled under reduced pressure to remove water and acetic acid. The residue is dissolved in 325 parts of 3% aqueous sodium hydroxide, filtered, neutralised with hydrochloric acid and extracted three times with 150 parts of chloroform. The chloroform solution is evaporated to dryness to yield 33 parts of pure 2-dimethylamino-4,5-dimethyl-6-hydroxy pyrimidine.

Provenance & Evidence