반응 #416404

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benzoyl chloride

triethyl phosphite

Ethyl chloride

→

diethyl benzoylphosphonate

수율 97.4%

반응 조건

후처리

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

실험 절차

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%).

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