DIMETHYL (1-HYDROXY-1-METHYLETHYL)PHOSPHONATE synthesis
- Product Name:DIMETHYL (1-HYDROXY-1-METHYLETHYL)PHOSPHONATE
- CAS Number:10184-68-6
- Molecular formula:C5H13O4P
- Molecular Weight:168.13
Yield:10184-68-6 91%
Reaction Conditions:
Stage #1: Dimethyl phosphite;acetonewith calcium fluoride for 0.0833333 h;
Stage #2: with potassium hydroxide at 40 - 50; for 5.16667 h;
Steps:
3
Add 33.015 g (0.30 mole) of dimethylphosphite and 22.651 g (0.39 mole) of acetone to a 100 ml 3-neck flask and add 4.685 g (0.06 mole) of calcium fluoride while stirring. After stirring for 5 minutes to confirm that calcium fluoride is well dispersed, 3.367 g (0.06 mole) of KOH is added over about 10 minutes. At this time, you can check the heat, but adjust the KOH feed rate so that the internal temperature does not exceed 55 °C. After the exothermic reaction is stopped, the internal temperature is adjusted to 45 °C and the reaction is stirred at an internal temperature of 40 to 50 °C for 5 hours. The completion of the reaction can be confirmed by TLC. After confirming the completion of the reaction, stirring is stopped, and 30 ml of methylene chloride is added while cooling to room temperature. As a result, the solid by-product is submerged on the bottom, and solid by-products can be removed by simple filtration. Thereafter, as in Example 1, the organic layer was washed with water, and methylene chloride was distilled off, followed by vacuum drying to obtain 45.9 g of the title compound. (Yield: 91.0%)
References:
KR2016/117684,2016,A Location in patent:Paragraph 0037; 0038
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