ChemicalBook CAS DataBase List Dimethyl acetylmethylphosphonate

Dimethyl acetylmethylphosphonate synthesis

13synthesis methods

Product Name:Dimethyl acetylmethylphosphonate
CAS Number:4202-14-6
Molecular formula:C5H11O4P
Molecular Weight:166.11

78-95-5

121-45-9

4202-14-6

General procedure for the synthesis of dimethyl acetone-based phosphonate from chloroacetone and trimethoxyphosphine: a dry and clean 500 mL coil was heated to 135 °C. 1000 g (0.7 eq., 10.81 mol) of chloroacetone (boiling point 117 to 119 °C at standard atmospheric pressure) was placed in charge bottle A and diluted with 4000 g of toluene. 1878 g (1.0 eq., 15.13 mol) of trimethoxyphosphine (boiling point at 112°C at standard atmospheric pressure) was placed in charge bottle B and diluted with 3122 g of toluene. After the temperature was stabilized, batch pumping of the chloroacetone-toluene solution in Bottle A and the trimethoxyphosphine-toluene solution in Bottle B was started at a rate of 12.5 g/min. The residence time of the reactants was 20 min, and the reaction pressure was maintained at 0.5 to 2.0 MPa. The reacted mixture was directly introduced into a thin-film evaporation unit, with a controlled pressure of 4 to 10 x 10^2 Pa and a temperature of between 60 and 70 °C. The reaction was carried out at a pressure of 4 to 10 x 10^2 Pa. Ultimately, 1230 g of dimethyl acetone-based phosphonate (boiling point 85 to 88 °C, 666 Pa) was obtained in 88% yield.

78-95-5
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$16.30/5 g

121-45-9
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$14.00/5g

4202-14-6
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$9.00/1g

Yield:4202-14-6 88%

Reaction Conditions:

in toluene at 135; under 3750.38 - 15001.5 Torr; for 0.333333 h;Large scale;Arbuzov Reaction;

Steps:

12 Example 12
The dry and clean 500mL coil was heated to 135 ° C, to take Compound 6 (standard atmospheric pressure boiling point of 117 to 119 ° C) 1000g (0.7eq.10.81mol) placed in a feeding bottle A, adding 4000g of toluene diluted trimethyl phosphite (standard large Pressure of boiling point 112 ° C) 1878g (1.0eq.15.13mol) placed in the bottle B, 3122g of toluene was added to be diluted to be coiled The batch was started after the temperature was stabilized, and pump A (toluene solution of compound 6): 12.5 g / min, pump B (trimethyl phosphite): 12.5 g / min. Residence time 20min, the reaction pressure is 0.5 ~ 2.0Mpa. The discharge port is directly connected to the thin-film evaporation device to control the pressure4 to 10 × 102 Pa and temperature of 60 to 70 ° C. Finally, 1230 g of product 7 (boiling point 85 to 88 ° C., 666 Pa) was obtained in a yield of 88%.

References:

Kailaiying Life Science And Technology (Tianjin) Co., Ltd.;Hong Hao;Zhan Musi·gaiji;Lu Jiangping;Li Chao;Zhang Enxuan CN107163079, 2017, A Location in patent:Paragraph 0076; 0077; 0078

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141-78-6 Synthesis