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Green synthesis method of methyl cyanoacetate

A technology of methyl cyanoacetate and green synthesis, which is applied in cyanide reaction preparation, carboxylic acid nitrile purification/separation, organic chemistry and other directions, can solve the problems of difficult wastewater treatment, low reaction yield, energy consumption, etc. The effect of avoiding solid waste, facilitating industrial production and saving production costs

Pending Publication Date: 2020-10-20
合肥全景泰益新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] After the neutralization reaction in the above-mentioned third step, vacuum distillation and dehydration are required, which consumes a large amount of energy. At the same time, centrifugation after dehydration produces a lot of sodium chloride with no industrial value, which causes a serious environmental burden.
[0008] Another method is to carry out cyanation reaction of methyl chloroacetate and sodium cyanide to prepare methyl cyanoacetate. In this method, sodium cyanide is a highly toxic substance, and the common raw material of sodium cyanide is 30% cyanide Sodium aqueous solution, the presence of water in the system will inhibit the reaction, the reaction yield is not high, and the generated wastewater contains CN - Pollution, wastewater treatment is difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh 28.35g of chloroacetic acid, measure 40ml of methanol (purity is 95wt%), mix and dissolve, add 0.5g of phosphotungstic acid to carry out esterification reaction at 90°C to prepare methyl chloroacetate, and pour the product into the reaction kettle after purification. Then add 26ml of acetone cyanohydrin to the reaction kettle, raise the system temperature to 40°C, continue the constant temperature reaction for 2.5h, recover the hydrogen chloride produced in the reaction with water, and distill out the acetone and unreacted acetone in the product after the reaction Cyanohydrin, the remaining product is purified by rectification to obtain methyl cyanoacetate, calculated as methyl chloroacetate, the yield is 65.3%.

Embodiment 2

[0032] Weigh 28.35g of chloroacetic acid, measure 40ml of methanol (purity is 95wt%), mix and dissolve, add 0.5g of phosphotungstic acid to carry out esterification reaction at 90°C to prepare methyl chloroacetate, and pour the product into the reaction kettle after purification. Then add 26ml of acetone cyanohydrin to the reaction kettle, raise the system temperature to 50°C, continue the constant temperature reaction for 2.5h, recover the hydrogen chloride produced in the reaction with water, and distill out the acetone and unreacted acetone in the product after the reaction Cyanohydrin, the remaining product is purified by rectification to obtain methyl cyanoacetate, and the yield is 82.5% based on methyl chloroacetate.

Embodiment 3

[0034] Weigh 28.35g of chloroacetic acid, measure 40ml of methanol (purity is 95wt%), mix and dissolve, add 0.5g of phosphotungstic acid to carry out esterification reaction at 90°C to prepare methyl chloroacetate, and pour the product into the reaction kettle after purification. Then add 26ml of acetone cyanohydrin to the reaction kettle, raise the system temperature to 70°C, continue the constant temperature reaction for 2.5h, recover the hydrogen chloride produced in the reaction with water, and distill out the acetone and unreacted acetone in the product after the reaction Cyanohydrin, the remaining product is purified by rectification to obtain methyl cyanoacetate, calculated as methyl chloroacetate, the yield is 90.3%.

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PUM

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Abstract

The invention discloses a green synthesis method of methyl cyanoacetate. The preparation process comprises the following steps: heating methyl chloroacetate and acetone cyanohydrin to 40-100 DEG C inthe absence of a catalyst and a solvent, and reacting to obtain methyl cyanoacetate. Acetone cyanohydrin serves as a cyaniding reagent and directly reacts with methyl chloroacetate to generate methylcyanoacetate, no other solvent or catalyst is needed, the yield is high, and the production cost is greatly reduced.

Description

technical field [0001] The invention relates to the technical field of organic green synthesis, in particular to a green synthesis method of methyl cyanoacetate. Background technique [0002] Methyl cyanoacetate is an intermediate in organic synthesis, medicine and dyes, mainly used in the manufacture of adhesives (such as medical adhesive 2-methyl cyanoacrylate), vitamin B6, malononitrile, etc., and is also an important component of pesticide synthesis. Intermediates, such as the preparation of 2-amino-4,6-dimethoxypyrimidine, can be used to prepare sulfonylurea herbicides. A kind of main synthetic method is the cyanoacetate esterification method at present, comprises the following steps, as formula (1-4): [0003] Neutralization reaction: 2ClCH 2 COOH+Na 2 CO 3 =2ClCH 2 COONa+CO 2 ↑+H 2 O (1) [0004] Cyanide reaction: ClCH 2 COONa+NaCN=CNCH 2 COONa+NaCl (2) [0005] Neutralization reaction: CNCH 2 COONa+HCl=CNCH 2 COOH+NaCl (3) [0006] Esterification reacti...

Claims

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Application Information

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IPC IPC(8): C07C255/19C07C253/14C07C253/34
CPCC07C253/14C07C253/34C07C255/19
Inventor 陈天云韩国井赵磊邱越刘文宏
Owner 合肥全景泰益新材料科技有限公司
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