How to synthesize Trimethyl phosphonoacetate?

Description

Phosphoryl 3-acetic acid methyl ester is a kind of chemical substance also known as phosphine acyl acetic acid trimethyl or Trimethyl phosphonoacetate, and its molecular formula is C5H11O5P. For the reaction of intramolecular Mannich type, generate sarain A type diaza tricyclic core; Oxa- for metal-organic catalysis, Michael reacts; Isoamyl alkene reaction for hydroxy indole and geranyl reaction; For intramolecular Horner-Wadsworth- Emmons reacts; For olefin cross metathesis/hetero-cyclization.

The chemical equation of this method is：

CH2ClCOOH+CH3OH→CH5ClO2+H2O

CH5ClO2+C3H9O3P→C5H11O5P+CH3Cl

Synthesis method

Step one: Methyl chloroacetate is obtained with methanol through esterification by monoxone.By methanol with monoxone by weight 0.366:1 mix homogeneously, agitating heating, carry out esterification at 105～110 DEG C.Monoxone is constantly steamed in course of reaction The ternary azeotrope of methyl ester, water, and methanol, through the layering of ester separator, the first separating alcohol and water is passed back in reaction pot again, The thick ester sodium carbonate neutralization separating, the crude product is dried to obtain methyl chloroacetate.

Step 2: The methyl chloroacetate crude product of step one proceeded to the synthesis reaction vessel, adds catalyst tetrabutylammonium iodide; it is heated to 80 DEG C, instills NSC 6513, rate of addition is controlled according to the backflow size of the reaction, backflow is bigger, Deca speed Degree is slower, controls interior temperature between 80～110 DEG C, time for adding controls and dripped off at 6～8 hours, then controls interior temperature 110～120 DEG C insulation 6～8 hours reaction, byproduct of reaction chloromethanes adopt deep cooling compress technique reclaim, obtain phosphine acyl acetic acid trimethyl Crude product. Methyl chloroacetate, catalyst, the weight of NSC 6513 are than for 1：0.02：1.1～1:0.02:1.2 between.

Step 3: The crude product of phosphine acyl acetic acid trimethyl is proceeded to purify a high-purity rectification tower. According to the material, boiling point, not with rectification, respectively, methyl chloroacetate (applied mechanically), organophosphorus fire retardant, and phosphine acyl acetic acid trimethyl go out. Rectifying still is residual, and proceed to special sell as phosphorus potash fertilizer after the alkali process in the reactor.

Phosphine acyl acetic acid trimethyl will pass through Michael Arbuzov with NSC 6513 and methyl chloroacetate for raw material Rearrangement reaction and be obtained. It is the technique of the production of esters product of domestic. Currently, most green environmental protection techniques have a higher conversion ratio, giving birth to techniques that prevent wastewater from being produced during production.

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