Dimethyl acetylmethylphosphonate

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.