Hydrochloric Acid → HCID 13369386, compound

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Reaction Steps

14.35 g. (0.05 mole) of 9-bromo-6-methyl-4-oxo-6,7,8,9-tetrahydro-4H-pyrido[1,2-a]pyrimidine-3-carboxylic acid are dissolved in 100 ml. of anhydrous chloroform. To the solution 15.0 ml. (0.15 mole) of n-butyl amine are added. The reaction mixture is allowed to stand for 3 days at room temperature, whereafter 70 ml. of water are added. The pH-value of the aqueous layer is adjusted under vigorous stirring to 2 by adding 10% by W/V hydrochloric acid solution. The organic layer is separated and the aqueous layer is shaken out with 2×50 ml. of chloroform. The combined organic layers are dried above calcinated sodium sulfate, finally the solvent is distilled off at reduced pressure. The residue is crystallized from methanol. 4.3 g. (31%) of 9-(n-butyl-amino)-6-methyl-4-oxo-6,7-dihydro-4H-pyrido[1,2-a]pyrimidine-3-carboxylic acid is obtained. Melting point: 13.5°-137° C.

Provenance & Evidence