Preparation method of dialkyl methylphosphonite

A technology of dialkyl methyl phosphinate and methyl phosphine dichloride is applied in the field of metal organic compound preparation, which can solve problems such as the decomposition of diethyl methyl phosphinate, achieve no three-waste discharge, improve efficiency, Safe and stable effect of reaction conditions
CN105949239AActive Publication Date: 2016-09-21庄建元
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
庄建元
Publication Date
2016-09-21
Patent Text Reader

Abstract

The invention relates to a preparation method of dialkyl methylphosphonite. tertiary amine with pKa greater than 10 is adopted as the acid binding agent, methyl phosphonic dichloride and alcohol react in a solvent, and the mole ratio of the methyl phosphonic dichloride, alcohol and tertiary amine is 1:2.0-2.4:2.0-2.4, the produced tertiary amine hydrochloride is neutralized with a caustic soda aqueous solution, and the solvent and tertiary amine obtained by evaporation is recycled and reused. The alkyl of the dialkyl methylphosphonite is straight chain and side chain alkane or alkene of aliphatic C1-C4, the alcohol refers to methanol, ethanol, propanol, isopropanol, allyl alcohol, n-butanol, isobutanol and the like, the tertiary amine refers to tertiary fatty amine, and also refers to fatty group and aromatic mixed tertiary amine, at the same time, the pKa of the tertiary amine is required to be greater than 10, and the tertiary amine can include triethylamine, tripropylamine and tributylamine.
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Description

technical field

[0001] The invention relates to a method for preparing dialkyl methylphosphonite, which belongs to the technical field of metal organic compound preparation. Background technique

[0002] Dialkyl methylphosphonite is an O,O-dialkylmethylphosphonite containing a phosphorus-carbon bond and is widely used in the preparation of flame retardants and herbicides.

[0003] DE 3,911,230 (Hoechst 1989) discloses that diethoxyphosphorous chloride is reacted with methylmagnesium halide in solvent tetrahydrofuran to obtain diethyl methylphosphonite through Grignard reaction,

[0004] (EtO)2PCl+MeMgBr→MeP(OEt)2+MgBr+MgCl yield 87.1%.

[0005] The more method is that MePCl2 (methyl phosphine dichloride) reacts with alcohol, and the hydrogen chloride produced is neutralized with an acid-binding agent.

[0006] MePCl2+2HOEt→MeP(OEt)2+2HCl

[0007] USP2,903,475 (Virginia Carolina Chem.Corp.1955) MePCl and pentane mixed solution are added dropwise in ethanol and pentane mixe...

Claims

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