Dimethyl acetylmethylphosphonate synthesis
- Product Name:Dimethyl acetylmethylphosphonate
- CAS Number:4202-14-6
- Molecular formula:C5H11O4P
- Molecular Weight:166.11
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
141-78-6
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4202-14-6
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4202-14-6
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4202-14-6
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