Acetic Acid → HCID 21278591, compound

Participants

Reaction Steps

240 mg of palladium at a concentration of 10% on calcium carbonate are added to 0.012 mole (4 g) of 4-chloro-2-(β,γ-dihydroxypropyl)amino-6-(β,γ-dihydroxypropyl)-aminonitrobenzene in 8.6 ml of triethylamine. 0.8 ml of acetic acid and 1.65 ml of formic acid are then added dropwise. The reaction mixture is heated under reflux for 7 hours. 10 ml of water are added. The reaction mixture diluted in this manner is filtered hot to remove the catalyst. The filtrate is evaporated to dryness under vacuum in the presence of absolute ethanol. The residue is dissolved in the minimum quantity of water. The expected product is extracted with ethyl acetate. The ethyl acetate phases are evaporated to dryness, after drying over sodium sulphate. After a small quantity of water has been added to the oil obtained, the expected product precipitates. Recrystallized from ethyl acetate, it melts at 138° C.

Provenance & Evidence