3,9-dichloro-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane 3,9-dioxide synthesis

Yield: 84%

Reaction Conditions:

with trichlorophosphate at 80 - 105; for 8 h;Temperature;

Steps:

3
34.04 g (0.25 mol) of pentaerythritol and 214.7 g (1.40 mol) of phosphorus oxychloride were added to a 250 ml four-necked flask equipped with a mechanical stirrer, a thermometer and a nitrogen condensate reflux tube. The oil bath was heated and refluxed. The reaction was carried out at 80 °C for 2h and the temperature was raised to 105 °C for 6 h. The unreacted phosphorus oxychloride was distilled off under reduced pressure, cooled, filtered, washed with dichloromethane, filtered and dried in vacuo at 70 °C to give pentaerythritol bisphosphate diphosphoryl chloride as a white powder in 84% yield.

References:

Sichuan University;Fan Haojun;Zhang Peikun;Tian Saiqi;Chen Yi;He Yazhou;Zhao Shiyu CN104497050, 2017, B Location in patent:Paragraph 0042; 0045; 0047-0048; 0051