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ChemicalBook CAS DataBase List Diphenyl chlorophosphate
2524-64-3

Diphenyl chlorophosphate synthesis

11synthesis methods
The preparation of Diphenyl chlorophosphate is as follows:With a thermometer,Reflux condenser and mechanical agitation120 g of dichloromethane was placed in a 500 ml four-neck reaction flask.7.3 g of N,N-dimethylformamide,Stirring temperature control below 10 °C,Put 28g of bis(trichloromethyl) carbonate,A solution of 50 g of diphenyl phosphate and 120 g of dichloromethane was added.After the addition, the reaction was carried out for 3 hours. After the end of the reaction, the temperature was controlled below 10 ° C, 20 g of water was slowly added, and the mixture was stirred and the organic phase was dried over anhydrous sodium sulfate. The desiccant was removed by filtration, and the filtrate was evaporated under normal pressure. The temperature was lowered to 0 ° C, and the insoluble matter was removed by filtration to obtain 48.9 g of diphenyl chlorophosphate. The purity of GC was 99.2%, and the yield was 90.3%.

2524-64-3.png

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Yield:2524-64-3 88.6%

Reaction Conditions:

with triphenylphosphine;Triphenylphosphine oxide;trichlorophosphate at 140; for 4 h;Large scale;

Steps:

4
1000 liter reactor were added 376 kg of phenol, 323 kg of phosphorus oxychloride and distillation primer in Example 3, the reaction was heated with stirring, over 4 hours temperature was raised to 140 ° C, the reaction was kept, in the GC controlling a phenol content of less than 0.5%, heat the reaction, the reaction liquid to the distillation column distillation, collecting 150 ± 2 ° C / 4mmHg fraction 475 kg namely finished diphenyl chlorophosphate, yield 88.6%, GC purity 99.3%.

References:

Changzhou Woteng Chemical Technology Co., Ltd.;Li Honggong;Chao Guoping;Sun Kezhou;Wang Huayun CN106810575, 2017, A Location in patent:Paragraph 0014

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