Manufacturing method of Ethyl tert-butyl acetophenone
Ethyl tert-butyl acetophenone (ETBPA) is an important raw material for the production of chemicals, which is widely used in the fields of pharmaceuticals, pesticides, and spices. This article will introduce a common manufacturing method of Ethyl tert-butyl acetophenone.
I. Raw materials and equipment
1. Raw materials: acetophenone, ethyl magnesium bromide, tert-butyl chloride.
2. Equipment: reaction kettle, condenser, dispensing funnel, stirrer, thermometer, pH meter and so on.
2. Manufacturing steps
1. Add appropriate amount of acetophenone and solvent in the reactor and stir well.
2. Prepare ethylmagnesium bromide in another container, and then add it slowly dropwise into the reaction kettle, control the dropwise acceleration, and keep the reaction temperature in a suitable range.
3. After completion of dropwise addition, continue stirring for some time to allow the reaction to proceed adequately.
4. Slowly add tert-butyl chloride dropwise into the reaction kettle, control the dropwise acceleration, and observe the change of reaction temperature and pH value at the same time.
5. After the dropwise addition, continue stirring for a period of time, and then leave to separate the layers.
6. Separate the organic layer, wash with water to neutral, then dry with anhydrous sodium sulfate.
7. The solvent is recovered by distillation and the crude product is obtained.
8. Refine the crude product, which can be done by recrystallization or distillation, etc., to obtain pure ethyl tert-butyl acetophenone.
3. Precautions
1. The reaction temperature and pH should be strictly controlled during operation to avoid side reactions.
2. The titration rate should be controlled when adding ethylmagnesium bromide and tert-butyl chloride to avoid too fast resulting in too violent reaction.
3. Attention should be paid to the operation specification during washing and drying to avoid product loss and contamination.
4. Suitable methods and conditions should be selected during the refining process to ensure the purity and yield of the product.
4. Safety and environmental protection
1. Attention should be paid to safety during operation, avoiding contact with fire and heat sources and avoiding inhalation and ingestion of products.
2. Waste should be properly disposed of to avoid harming the environment and human body.
All in all, the manufacture of ethyl tert-butyl acetophenone needs to strictly follow the operating procedures and safety and environmental protection requirements to ensure the quality and yield of the product, and at the same time reduce the production cost and improve the economic and social benefits of the enterprise.
