Reacción #416404

ord-4b143721646d4431b493c2337d58561b

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe unreacted benzoyl chloride and triethyl phosphite were removed by distillation at reduced pressure, terminal conditions
  2. 2
    Otrobeing 100° C

Procedimiento

To 140.57 grams (1.0 mole) of benzoyl chloride at 90° C there were added 166.2 grams (1.0 mole) of triethyl phosphite over a period of 1 hour. Ethyl chloride evolution ceased at the end of this period. The unreacted benzoyl chloride and triethyl phosphite were removed by distillation at reduced pressure, terminal conditions being 100° C and 8 mm, leaving a residue of 236 grams (90% yield) of diethyl benzoylphosphonate which was reacted with diethyl sodium phosphite as in Example 1 to produce tetraethyl phenyl hydroxymethane diphosphonate. This was hydrolyzed and the hydrolysis product purified in the same manner as in Example 1 to produce phenyl hydroxymethane diphosphonic acid as a viscous syrup having an acid number of 822 mg KOH/mg (Theroy is 835 mg KOH/gm); % P 22.8 (Theory 22.9%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04020091uspto-grants-1977_04