Formic Acid → HCID 86736770, compound

Participants

Reaction Steps

Formic acid (2.0 ml.) was added dropwise to acetic anhydride (2.45 g.) at ambient temperature with stirring. After the stirring was continued at the same temperature for 30 minutes, 3-(N-hydroxyamino)propylphosphonic acid (3.10 g.) was added to the mixture. The reaction mixture was stirred for an hour and concentrated under reduced pressure to give a residue, which was dissolved in water (25 ml.). To the aqueous solution was added ethylenediamine (0.60 g.). The mixture was concentrated under reduced pressure to give a residue, which was dissolved in water. The aqueous solution was concentrated under reduced pressure to give a residue, and to the residue was added ethanol (30 ml.) to give crystals. The crystals were separated by filtration and washed twice with ethanol (10 ml.) to give crystalline ethylenediamine bis[3-(N-formyl-N-hydroxyamino)propylphosphonate] (3.95 g.), a part (3 g.) of which was recrystallized from 90% aqueous methanol to give needles (1 g.) of the same object compound. M.p. 112°-118° C.

Provenance & Evidence