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The manufacturing method
of butyl ethyl cyanoacetate
1. Introduction
Butyl ethyl cyanoacetate is an important organic synthesis intermediate, widely used in the production of pharmaceuticals, pesticides, dyes and other chemicals. The purpose of this paper is to introduce the manufacturing method of ethyl butyl cyanoacetate and provide reference for its production.
2. Materials and Equipment
1. Materials: n-butanol, ethyl cyanoacetate, sodium sulfate, sodium hydroxide, toluene, etc.
2. Equipment: reaction kettle, separatory funnel, condenser, stirrer, thermometer, pH meter, etc.
3. manufacturing method
1. synthesis reaction
in the reaction kettle to add a certain amount of n-butanol and ethyl cyanoacetate, heating to a certain temperature, stirring for a certain period of time, so that the two fully react, generating butyl ethyl cyanoacetate.
reaction equation: CH3(CH2)3OH CH3CNCOOC2H5 → CH3(CH2)3OCOCH2CN C2H5OH
2. Neutralization reaction
After the synthesis reaction is completed, sodium sulfate is added to the reaction solution to react with the remaining sodium hydroxide and neutralize to neutrality.
3. Extraction and Separation
Toluene was added to the neutralized reaction solution, and the mixture was stirred for a certain period of time to sufficiently dissolve ethyl butylcyanoacetate in toluene. Then, the layer was separated by standing, and the lower aqueous solution was separated by a separatory funnel to obtain an upper organic phase.
4. Distillation and purification
The organic phase was distilled to collect fractions in a certain temperature range to obtain ethyl butyl cyanoacetate with high purity.
4. precautions
1. During the synthesis reaction, it is necessary to strictly control the temperature and stirring speed to ensure the smooth progress of the reaction.
2. During the neutralization reaction, it is necessary to control the amount of sodium sulfate added to avoid excessive loss of ethyl butyl cyanoacetate.
3. In the extraction process, it is necessary to select the appropriate solvent to ensure the full dissolution and separation of ethyl butyl cyanoacetate.
4. During the distillation process, it is necessary to control the distillation temperature and the range of collected fractions to ensure the purity of the product.
5. Conclusion
High purity ethyl butyl cyanoacetate can be obtained by the manufacturing method described in this paper. In the actual production process, it is necessary to adjust and optimize the operating parameters according to the specific situation to improve the quality and yield of the product. At the same time, it is necessary to pay attention to the safety and environmental protection issues in the production process to ensure the smooth progress of production.