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14337-77-0

Phosphinic acid, P,P-dimethyl-, methyl ester synthesis

10synthesis methods
-

Yield:14337-77-0 95%

Reaction Conditions:

at 120; for 4 h;Inert atmosphere;

Steps:

1 Example 1 Preparation of methyl dimethylphosphinate

In a 1L reactor equipped with condensing reflux device, dripping device and nitrogen gas, 2mol of reducing agent phenylsilane is added, 3mol of dimethyl methylphosphonate is added dropwise at 5, and the temperature is gradually increased to Keep at 90°C for about 1 hour, and then subtractively distill under a nitrogen atmosphere to obtain the product, dimethyl methyl phosphonite, with a yield of about 92% (wt). Then, in a reactor equipped with a reflux device, a dripping device and nitrogen gas, the compound methyl dimethyl phosphonite is added, the halogenated hydrocarbon methyl iodide is added dropwise, and the temperature is raised to 120°C, and the reaction is refluxed for 4 hours. Under reduced pressure distillation, the product methyl dimethyl hypophosphite was obtained, and the yield was about 95% (wt).

References:

CN112321638,2021,A Location in patent:Paragraph 0049-0050