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Synthesis method of ethyl cyanoacetate

A technology of ethyl cyanoacetate and cyanoacetic acid is applied in the synthesis field of ethyl cyanoacetate, can solve the problems of difficulty in separation, increased side reactions, low conversion rate in the reaction process, etc., and achieves the effects of reducing side reactions and improving product yield

Inactive Publication Date: 2018-12-18
营创三征(营口)精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the synthesis process, there are the following two problems: 1) Since the esterification reaction is a reversible reaction, the conversion rate of the reaction process is relatively low, resulting in a large amount of unreacted raw materials in the product, which brings certain difficulties to the separation and increases the separation cost.
2) The water generated by the esterification reaction will slowly generate carboxylic acid with the cyano group in ethyl cyanoacetate under the action of sulfuric acid, resulting in increased side reactions

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] A kind of synthetic method of ethyl cyanoacetate, the steps are as follows:

[0013] Add cyanoacetic acid to ethanol to dissolve, control the molar ratio of cyanoacetic acid to ethanol to be 1:3, transfer to the reaction kettle after dissolving. Stirring, under room temperature conditions, slowly add 98% concentrated sulfuric acid to the reactor from the dropping funnel, control the mass ratio of cyanoacetic acid to sulfuric acid to 1:0.08, control the temperature at 55 °C, and control the temperature of the system at 85 °C after the addition is completed. ℃, drop concentrated sulfuric acid and feed sulfur trioxide into the feed solution at a constant speed, control the molar ratio of cyanoacetic acid to sulfur trioxide to be 1:0.4, and the reaction ends after reflux for 4 hours.

[0014] At 80°C, the ethanol component in the reaction system was distilled under normal pressure, and 12% ammonia water was added dropwise to the system for neutralization, the temperature wa...

Embodiment 2

[0016] A kind of synthetic method of ethyl cyanoacetate, the steps are as follows:

[0017] Add cyanoacetic acid to ethanol to dissolve, control the molar ratio of cyanoacetic acid to ethanol to be 1:4, transfer to the reaction kettle after dissolving; stir, and slowly add 98wt.% concentrated sulfuric acid to the reactor from the dropping funnel under room temperature conditions , control the mass ratio of cyanoacetic acid to sulfuric acid to be 1:0.2, and control the temperature to be 65°C. After the dropwise addition, raise the system temperature to 70°C, add the concentrated sulfuric acid dropwise and feed sulfur trioxide at a uniform speed into the feed liquid at the same time, control The molar ratio of cyanoacetic acid to sulfur trioxide is 1:0.1, and the reaction is completed after reflux for 4 hours; under the temperature condition of 85°C, the ethanol component in the reaction system is distilled out under normal pressure, and 12wt.% ammonia water is added dropwise to ...

Embodiment 3

[0019] A kind of synthetic method of ethyl cyanoacetate, the steps are as follows:

[0020] Add cyanoacetic acid to ethanol to dissolve, control the molar ratio of cyanoacetic acid to ethanol to be 1:4, transfer to the reaction kettle after dissolving; stir, and slowly add 98wt.% concentrated sulfuric acid to the reactor from the dropping funnel under room temperature conditions , control the mass ratio of cyanoacetic acid to sulfuric acid to be 1:0.2, and control the temperature to be 55°C. After the dropwise addition, raise the system temperature to 70°C, add concentrated sulfuric acid dropwise and simultaneously feed sulfur trioxide into the feed liquid at a uniform speed to control The molar ratio of cyanoacetic acid to sulfur trioxide is 1:0.1, and the reaction ends after reflux for 4 hours; under the temperature condition of 80°C, the ethanol component in the reaction system is distilled out under normal pressure, and 12wt.% ammonia water is added dropwise to the reaction...

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PUM

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Abstract

The invention belongs to the technical field of organic synthesis, and provides a synthesis method of ethyl cyanoacetate. During the process of esterification reactions, sulfur trioxide is slowly introduced and reacts with water generated by the esterification reactions to generate sulfuric acid; sulfur trioxide is taken as a catalyst to promote the reactions to move to the right direction, at thesame time, water is consumed, the side reactions are prevented, the product yield is increased, and the happening rate of side reactions is reduced.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a synthetic method of ethyl cyanoacetate. Background technique [0002] Ethyl cyanoacetate is an intermediate of fine chemical products such as pharmaceuticals and dyes, and is used in the synthesis of esters, amides, acids, and nitriles. In Japan, it is mainly used as an intermediate of cyanoacrylate quick-drying adhesives, used in the bonding of auto parts and household appliances assemblies, and also used in vitamin B6, synthetic dyes and other fields. The cyclization of ethyl cyanoacetate with methoxyacetylacetone and ammonia can produce 5-cyano-6-hydroxy-4-methoxymethyl-2-picoline. After nitration, chlorination and catalytic hydrogenation, 3-amino-5-aminomethyl-4-methoxymethyl-2-picoline can be obtained. Further diazotization, hydrolysis, and salt formation can obtain vitamin B6. [0003] At present, the synthesis of ethyl cyanoacetate is mainly base...

Claims

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Application Information

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IPC IPC(8): C07C255/19C07C253/30C07C253/34
CPCC07C253/30C07C253/34C07C255/19
Inventor 刘至寻梁海赵志刚
Owner 营创三征(营口)精细化工有限公司
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