Hydrochloric Acid → HCID 19834637, compound

Participants

Reaction Conditions

Reaction Steps

The mixture consisting of 8.5 g of ammonium acetate, 7.5 g of 10% palladium on charcoal, 0.05 mole (15 g) of 5-methylamino-3-amino-2,4-dimethoxychlorobenzene hydrochloride in 14 ml of water containing 90 ml of ethanol and 15.2 g of triethylenediamine, was heated to 70° C. with stirring, and then 6.44 g of formic acid were added dropwise. Heating was maintained for 1 hour after completion of the addition. The catalyst was removed by filtration. The solids content obtained by evaporation of the filtrate under vacuum was dissolved in ethyl acetate. A 7N hydrochloric acid solution in absolute ethanol was added to the ethyl acetate which had been dried over sodium sulphate, in order to precipitate the expected product. The latter was recrystallized while hot from an aqueous-alcoholic solution of hydrochloric acid.

Provenance & Evidence