59360-02-0Relevant articles and documents
Purification method of dialkyl methylphosphite
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Paragraph 0044-0046; 0053-0058; 0068-0073, (2020/12/15)
The invention relates to the technical field of compound purification, and particularly provides a purification method of dialkyl methylphosphite. The purification method comprises the following steps: adding a weak polar solvent into a reaction solution containing dialkyl methylphosphite, magnesium chloride and an ether solvent, conducting cooling to -10 DEG C to 40 DEG C, adding a nitrogen-containing organic alkali compound, carrying out a heat preservation reaction, and conducting filtering to obtain magnesium chloride and a filtrate; and rectifying the filtrate to obtain a dialkyl methylphosphite product. According to the purification method provided by the invention, the purity and the yield of the dialkyl methylphosphite are improved, the obtained magnesium chloride does not containcrystal water, the nitrogen content in the magnesium chloride is 0.01-0.5%, and the purity of the anhydrous magnesium chloride can reach 97% or above; and the purity of the obtained dialkyl methylphosphite product can reach 97% or above, and the yield can reach 85% or above. The method has the advantages of simple process, no need of special equipment, mild reaction conditions and no need of high-temperature distillation or low-temperature brine treatment process, and is suitable for large-scale industrial production.
Direct α-chlorination of O,O-dialkyl chalcogenophosphonates with phosphorus oxychloride
Mons, Stéphane,Sabourault, Nicolas,Klein, Emmanuel,Mioskowski, Charles,Lebeau, Luc
, p. 7547 - 7549 (2007/10/03)
α-Chlorination of phosphonates, and O,O-dialkyl thio- and selenophosphonates involving the direct reaction of their lithiated anion with phosphorus oxychloride is described. The reaction gives good results where previously known methods fail. The role of the chalcogen atom, and the influence of the nature of the alkyl chain with respect to the reactivity are discussed.