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Preparation method of triethyl phosphonoacetate

A technology of triethyl phosphoroacetate and triethyl phosphite, which is applied in the field of preparation of triethyl phosphoroacetate, can solve the problems of low purity, high production cost, and low yield, and achieve high purity and low cost. Low, high yield effect

Pending Publication Date: 2022-02-25
TAICANG YUNTONG BIOCHEM ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of this method is low, and the purity is not high, and the cost for industrial production is relatively high

Method used

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  • Preparation method of triethyl phosphonoacetate
  • Preparation method of triethyl phosphonoacetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 3mol phenethyl ether and 1mol triethyl phosphite into the reaction kettle, then raise the temperature to 120°C, slowly add 1mol ethyl chloroacetate dropwise, the released ethyl chloride will co-produce ethyl chloride in the absorption tank; add chloroacetic acid dropwise Ethyl ester was kept at 120°C for 3h. Nitrogen gas was introduced into the reaction kettle for 1h, and the ethyl chloride was driven off to make the reaction complete. The material is pumped into a distillation pot, and distilled under reduced pressure at 150°C. The first fraction is collected, mainly raw materials and phenetole, and the later fraction is collected at 500 Pa and 150°C, monitored by gas chromatography, and the finished product is obtained.

[0026] Add 3mol sodium phenoxide solution into the absorption kettle to capture ethyl chloride from the upper reaction kettle, keep the temperature of the absorption kettle at 80°C, cool and separate the layers after absorption, pump the oil laye...

Embodiment 2

[0028] Add 2mol phenethyl ether and 1mol triethyl phosphite into the reaction kettle, then raise the temperature to 130°C, slowly add 2mol ethyl chloroacetate dropwise, the released ethyl chloride will co-produce ethyl chloride in the absorption tank; add chloroacetic acid dropwise Ethyl ester was kept at 120°C for 3h. Nitrogen gas was introduced into the reaction kettle for 2h, and the ethyl chloride was driven out to make the reaction complete. The material is pumped into a distillation pot, and distilled under reduced pressure at 150°C. The first fraction is collected, mainly raw materials and phenetole, and the later fraction is collected at 500 Pa and 140°C, monitored by gas chromatography, and the finished product is obtained.

[0029] Add 4mol sodium phenoxide solution into the absorption kettle to capture the ethyl chloride escaped from the upper reaction kettle, keep the temperature of the absorption kettle at 75°C, cool and separate the layers after absorption, pump ...

Embodiment 3

[0031] Add 4mol phenethyl ether and 1mol triethyl phosphite into the reaction kettle, then raise the temperature to 130°C, slowly add 3mol ethyl chloroacetate dropwise, the released ethyl chloride will co-produce ethyl chloride in the absorption tank; add chloroacetic acid dropwise Ethyl ester was kept at 125°C for 4h. Nitrogen gas was introduced into the reaction kettle for 1h, and the ethyl chloride was driven off to make the reaction complete. The material is pumped into a distillation kettle, and distilled under reduced pressure at 150°C. The first fraction is collected, mainly raw materials and phenetole, and the later fraction is collected at 600 Pa and 150°C, monitored by gas chromatography, and the finished product is obtained.

[0032] Add 6mol sodium phenoxide solution into the absorption kettle to capture the ethyl chloride escaped from the upper reaction kettle, keep the temperature of the absorption kettle at 75°C, cool and separate the layers after absorption, pu...

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Abstract

The invention belongs to the field of chemical synthesis, and particularly relates to a preparation method of triethyl phosphonoacetate. The preparation method comprises the following steps of: mixing phenetole and triethyl phosphite, dropwise adding ethyl chloroacetate at high temperature, and reacting to obtain triethyl phosphonoacetate. Meanwhile, chloroethane generated by the reaction reacts with excessive sodium phenate to obtain phenetole. Triethyl phosphonoacetate and phenetole are prepared by the method, the yield is high, the method is simple, the price is low, the controllability is good, the prepared phenetole can be used as a front-end raw material, redundant phenetole can be sold, the preparation cost is greatly saved, and the method has an application prospect in the field of chemical synthesis.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a preparation method of triethyl phosphoroacetate. Background technique [0002] Triethyl phosphite, the chemical formula is C 6 h 15 o 3 P, colorless and transparent liquid, insoluble in water, easily soluble in organic solvents such as ethanol and ether, will be hydrolyzed into diethyl phosphite after a long time in water. It can be used as plasticizer, lubricating oil additive and stabilizer. [0003] Ethyl chloroacetate, the structural formula is ClCH 2 COOC 2 h 5 , Colorless transparent liquid with a pungent pungent odor, decomposed in hot water or alkali, miscible with ethanol and ether, insoluble in water. The freezing point is -26°C. It is often used as a raw material for pharmaceuticals and spices, and can also be used as a solvent. [0004] The chemical formula of phenetole is C 8 h 10 O, colorless oily liquid with aromatic odor. Melting point -3...

Claims

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Application Information

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IPC IPC(8): C07F9/40
CPCC07F9/4075C07F9/4006
Inventor 张伟栋
Owner TAICANG YUNTONG BIOCHEM ENG
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