Manufacturing method of ethyl butylcyanoacetate
I. INTRODUCTION
Ethyl butylcyanoacetate is an important organic synthesis intermediate, which is 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 butylcyanoacetate for its production.
II. Materials and equipment
1. Materials: n-butanol, ethyl cyanoacetate, sodium sulfate, sodium hydroxide, toluene and so on.
2. Equipment: reaction kettle, dispensing funnel, condenser, stirrer, thermometer, pH meter and so on.
3. Manufacturing method
1. Synthetic reaction
Add a certain amount of n-butanol and ethyl cyanoacetate in the reaction kettle, heat to a certain temperature, stir for a certain period of time, so that the two are fully reacted to produce butyl ethyl cyanoacetate.
Reaction equation: CH3(CH2)3OH + CH3CNCOOC2H5 → CH3(CH2)3OCOCH2CN + C2H5OH
2. Neutralization reaction
After the synthesis reaction is completed, sodium sulphate is added to the reaction solution to react with the remaining sodium hydroxide and neutralize to neutral.
3. Extraction and Separation
Toluene was added to the neutralized reaction solution and stirred for a certain time to fully dissolve ethyl butylcyanoacetate in toluene. Then leave to separate the layers, the lower layer of aqueous solution is separated out by a separatory funnel, and the upper layer of organic phase is obtained.
4. Distillation and purification
The organic phase is distilled, and the fractions in a certain temperature range are collected to obtain ethyl butylcyanoacetate with higher purity.
4. Precautions
1. During the synthesis reaction, the temperature and stirring speed need to be strictly controlled to ensure the smooth progress of the reaction.
2. During the neutralization reaction, the amount of sodium sulfate added needs to be controlled to avoid the loss of butylcyanoacetic acid ethyl ester due to excess.
3. In the extraction process, it is necessary to choose appropriate solvents to ensure the full dissolution and separation of ethyl butylcyanoacetate.
4. During distillation, the distillation temperature and the range of collected fractions need to be controlled to ensure the purity of the product.
V. CONCLUSION
By the manufacturing method described in this paper, ethyl butylcyanoacetate with high purity can be obtained. In the actual production process, the operating parameters need to be adjusted and optimized according to the specific conditions in order to improve the quality and yield of the product. At the same time, attention needs to be paid to the safety and environmental protection in the production process to ensure the smooth progress of production.
