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[Chemical Knowledge]：Production method and process of ethyl propyl cyanoacetate

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The manufacturing method
of ethyl propyl cyanoacetate
1. Introduction

Ethyl propyl cyanoacetate is an important chemical raw material, which is widely used in medicine, pesticide, plastic and other fields. This article will introduce the manufacturing method of propyl cyanoacetate in detail, including raw material preparation, reaction steps, post-treatment and precautions.

2. Raw Material Preparation

1. Propyl cyanide: Propyl cyanide is the main raw material for the preparation of ethyl propyl cyanoacetate, which is generally prepared by the addition reaction of acrylonitrile and hydrogen.
2. Ethyl chloroacetate: Ethyl chloroacetate, as another raw material, can be prepared by esterification of chloroacetic acid with ethanol.

3. Reaction Procedure

1. In a reaction kettle equipped with a stirrer, a thermometer and a reflux condenser, a measured amount of propyl cyanide and ethyl chloroacetate is added.
2. Open the stirring, heat the reaction kettle to a certain temperature, and maintain a constant temperature reaction for a certain period of time.
3. The progress of the reaction was monitored by thin layer chromatography (TLC) and when the starting material was completely reacted, the heating was stopped.
4. Cool the reaction vessel to room temperature, transfer the reaction solution to a separatory funnel, wash several times with water, and discard the aqueous phase.
5. The organic phase was dried over anhydrous sodium sulfate, and the drying agent was removed by filtration to obtain ethyl propyl cyanoacetate as a crude product.

4. post-treatment

1. the crude propyl cyanoacetate is transferred to a distillation kettle and subjected to atmospheric distillation to collect the target fraction.
2. The fine propyl cyanoacetate obtained by distillation is sealed with a brown reagent bottle to avoid light and high temperature.

5. Precautions

1. Propyl cyanide and ethyl chloroacetate are toxic chemicals. During operation, laboratory safety regulations must be strictly observed and protective equipment must be worn.
2. Keep constant temperature during the reaction to avoid too high or too low temperature affecting the reaction speed and selectivity.
3. When washing the organic phase with water, the water temperature should be controlled to avoid the hydrolysis of ethyl propyl cyanoacetate.
4. During the drying process, it is necessary to ensure that the anhydrous sodium sulfate is completely dried to avoid moisture being brought into the subsequent distillation steps.
5. The heating speed should be controlled during distillation to avoid local overheating and product decomposition.

6. Conclusion

Through the above steps, we can successfully prepare ethyl cyanoacetate. In the actual operation process, the laboratory safety regulations should be strictly observed, and the operation steps should be adjusted according to the specific experimental conditions to ensure the purity and yield of the product. The manufacturing method described in this paper is the basic reference, and the specific experimental operation should be carried out under the guidance of professionals.

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