1184-10-7

139-02-6

1184-10-7

The general procedure for the synthesis of phenoxycyclotriphosphonitrile from sodium phenol was as follows: 1000 g of acetonitrile was added to the reaction vessel and cooled to 30°C using a solid funnel. 120 g (0.345 mol) of hexachlorocyclotriphosphonitrile was slowly added, and the dosing process lasted for 1 hour, with a final temperature control of 45°C. Subsequently, the reaction was heated to 80°C to start refluxing and the residual amount of hexachlorocyclotriphosphonitrile was confirmed to be 0.20% after the reaction had been completed by HPLC after 4 hours. After 4 hours the reaction was confirmed to be complete by HPLC with a residue of 0.20% HCTN. The acetonitrile was firstly distilled at atmospheric pressure to remove the acetonitrile, the distillation process should be carried out slowly, and then vacuum distillation was carried out under slow decompression to recover 980 g of acetonitrile. The remaining acetonitrile was evaporated by adding 2% sodium hydroxide solution, and 600 ml of toluene obtained from step 1 was heated to 55°C with stirring for 1 hour, and the aqueous layer was separated. The final product was washed with 600 ml of 5% sodium chloride solution and 600 ml of pure water, respectively, and the final product was washed in layers using the same method to obtain the toluene solution. Toluene was distilled under reduced pressure and a total of 490 g of toluene was recovered.After distillation of the toluene, 300 g of anhydrous ethanol was added to the residue, heated and refluxed for 1 h, cooled to 20°C and kept for 1 h, and centrifuged. Finally, it was dried at 60°C for 5 hours to obtain 228g of white hexaphenoxycyclotriphosphonitrile with 99.25% purity by HPLC, 95.24% yield and 100 ppm chlorine ion.