Perchloric Acid → HCID 21437984, compound

Participants

Reaction Steps

6 gm (0.02 mol) of 4-(2'-nitro-4-biphenylyl)-4-oxo-butyric acid were hydrogenated in 60 ml of acetic acid and 2.5 ml of perchloric acid in the presence of 2.5 gm of palladium/barium sulfate (5%) as catalyst at room temperature and at a pressure of 5 atmospheres in a Parr-autoclave. After absorption of the calculated quantity of hydrogen, the catalyst was vacuum-filtered off, and the solvent was removed in vacuo. The residue was dissolved in water and admixed with ether. By addition of sodium bicarbonate solution, the aqueous phase was adjusted to a pH-value of about 5. Now, the ether solution was separated, washed with water and the solvent was removed. The obtained 4-(2'-amino-4-biphenylyl)-butyric acid was dissolved in ether and mixed with cyclohexylamine; the precipitated cyclohexylamine salt was collected and recrystallized from methylene chloride and then from acetone/ether. Melting point 123°-126° C.

Provenance & Evidence