Diethylamine → 1,1-Di(phosphonic acid diethyl ester)-1-hydroxy ethane

Participants

Reaction Steps

Diethyl hydrogen phosphite (1.0 mole) and diethyl amine (1.0 mole) were combined in a round bottom flask. Diethyl acetylphosphonate (1.0 mole) was added dropwise, with stirring. The reaction mixture was maintained at a temperature of about 75° C. for an additional 2 hours after all of the diethyl acetyl phosphonate was added. The resulting mixture was distilled under reduced pressure to yield tetraethyl 1-hydroxyethylidene bisphosphonic acid as a pale yellowish liquid which crystallized at -15° C. into small needle-shaped crystals.

Provenance & Evidence