Sulfuric Acid → HCID 19357420, compound

Participants

Reaction Steps

150 ml of methanol were introduced into a 0.3 liter autoclave, 16.7 g (0.2 mole) of N,N'-bis-(2,5-dinitrophenyl)-1,2-diaminoethane were dissolved therein and 2 g of palladium on active carbon 10% (Degussa) were added. After the autoclave had been closed and blanketed with nitrogen, hydrogenation was carried out under a pressure of 3 bar and at a temperature of 35 to 40° C. until no more hydrogen was taken up. The mixture was emptied onto a pressure filter, the residue was dissolved in 100 ml of N-methyl pyrrolidone at 100° C., the catalyst was filtered off using a pressure filter and, after cooing of the filtrate to 5-10° C., 9.8 g (0.1 mole) of 80% sulfuric acid were added dropwise. The jelly-like precipitate was stirred with 200 ml of methanol. The crystallized product was filtered off under suction, washed with methanol and dried.

Provenance & Evidence