反应详情

温度

100 °C

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%.

1. temperatureReflux
2. temperatureis maintained for a further 5 hours
3. distillationThe excess phosphorus trichloride is distilled off at 120° C. in vacuo
4. addition966 g of toluene are added
5. temperatureCooling to room temperature