The preparation of diethyl malonate
diethyl malonate is also an important agent for organic synthesis. The preparation method is related to all kinds of chemical principles, and the operation skills need to be refined.
Start by taking an appropriate amount of chloroacetic acid, dissolve it in water, and slowly drop it into the soda ash solution, during which the temperature of the reaction is controlled, so as not to overplay. Chloroacetic acid and soda ash phase combine, sodium chloroacetate, this step should be stable and uniform, so that the reaction is sufficient.
Next, add sodium cyanide to the obtained sodium chloroacetate solution. Sodium cyanide is highly toxic, and it should be done with caution. When the two come into contact, a nucleophilic substitution reaction occurs, and sodium cyanoacetate is produced. This reaction must be carried out in a closed vessel and at a moderate temperature to prevent the escape of sodium cyanide and endanger the human body.
When sodium cyanoacetate is formed, it is dissolved in ethanol, and then sulfuric acid is added to perform an esterification reaction. Catalyzed by sulfuric acid, sodium cyanoacetate is phased with ethanol to gradually produce diethyl malonate. During the reaction, observe its color and smell its smell to judge the process.
After the reaction is completed, purify it by distillation. Initially filter out impurities, then put it into a still, control the temperature near the boiling point of diethyl malonate, and collect its fraction. The distilled product is clear and has a special fragrance, which is diethyl malonate.
To prepare diethyl malonate, every step is heavy, from the choice of raw materials, to the control of the reaction, to the purity of the product, which is interlinked and cannot be lost. The subtle secrets of chemistry can be seen here.