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ChemicalBook CAS DataBase List Trimethyl phosphate

Trimethyl phosphate synthesis

13synthesis methods
Trimethyl phosphate is prepared by treating phosphorus oxychloride with methanol in the presence of an amine base:
POCl3 + 3 CH3OH + 3 R3N → PO(OCH3)3 + 3 R3NH+Cl
It is a tetrahedral molecule that is a weakly polar solvent.
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Yield:512-56-1 97.5%

Reaction Conditions:

with trichlorophosphate in acetone at 10 - 30; under 10 Torr; for 4 h;

Steps:

7 Example 7

In a 2L to of the three-port flask 260.2g, 8mol methanol, then adding acetone 92.9g, 1 . 6mol, after stirring and mixing cooling to 10 °C the following, stirring next adds by drops 245.33g, 1 . 6mol phosphorus oxychloride, control the mixture temperature is not higher than 10 °C. 50 minutes after the dropping. Stirring 10 minutes, under the condition of vacuum heating to 30 degrees, the vacuum degree 10mmHg, reaction 3h, the end of the reaction, adding containing 8.5g methanol the sodium is mellow solution, stirring for one hour, water after cooling, dissolve, produce sodium chloride, separating, collecting the organic phase, the organic phase washed to neutral, moisture is removed by reduced pressure distillation and low-boiling methanol and acetone, the purity is not less than 96% triethyl phosphate product the ester is thick 292.4g, the fractionating column, pressure reducing fractionated 218.5g methyl phosphate, yield 97.5%, purity ≥ 99.5%.

References:

CN105859770,2016,A Location in patent:Paragraph 0042; 0043

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