Reaktion #362267

Reaktionsgleichung

o-phenylphenol

phosphorus trichloride

hydrogen chloride

→

6-chloro-(6H)-dibenz[c,e][1,2]oxaphosphorin

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturReflux
2. 2
   Temperaturis maintained for a further 5 hours
3. 3
   workup.DISTILLATIONThe excess phosphorus trichloride is distilled off at 120° C. in vacuo
4. 4
   workup.ADDITION966 g of toluene are added
5. 5
   TemperaturCooling to room temperature

Vorschrift

700 g (4.12 mol) of o-phenylphenol and 4.1 g of zinc chloride are heated to 180° C. with stirring. 692 g (5.03 mol) of phosphorus trichloride are then added dropwise over 12 hours. Reflux is maintained for a further 5 hours; at the end no further hydrogen chloride is evolved. The excess phosphorus trichloride is distilled off at 120° C. in vacuo, the reaction product is cooled to 100° C. and 966 g of toluene are added. Cooling to room temperature gives a 50% strength solution of 6-chloro-(6H)-dibenz[c,e][1,2]oxaphosphorin in toluene. The 31P-NMR spectrum indicates a purity of 95.5%.

Quelle