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[Chemical Knowledge]：Production process and preparation method of isophorone IP

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Isophorone IP is a widely used organic synthesis intermediate. Many drugs and chemicals are prepared from isophorone IP. Therefore, the production process and preparation method are of great concern. Especially in the pharmaceutical industry, the content and purity of isophorone IP have an important influence on the quality and efficacy of the drug. This article will introduce the production process and preparation method of isophorone IP, hoping to provide a useful reference for the industry.
1. Production process of isophorone IP
There are two main production processes of isophorone IP, namely, epoxidation and o-hydroxyacetophenone oxidation.
1.1 epoxidation method
epoxidation method is through the epoxidation of o-hydroxyacetophenone, and then through the reduction of decomposition to obtain isophorone IP. The specific process is as follows:
Preparation of raw materials: o-hydroxyacetophenone is used as raw material, sodium hydroxide and propylene oxide are added, and the reaction is carried out at about 30 ° C. for 10 hours. Epoxidized o-hydroxyacetophenone is obtained. Decomposition and reduction of
: the reaction product is added to a mixed solution of ethanol and sodium hydroxide, and heated under constant stirring. The decomposition and reduction reaction will produce isophorone IP, and produce certain by-products, such as 4-(3-hydroxy-3-methylpropyl) phenol, etc., which need to be further distilled and purified to obtain pure isophorone IP.
The advantages of this process are that the raw materials are readily available and can be produced on a large scale. But the disadvantage is that a certain by-product is produced, which needs to be purified many times to obtain pure isophorone IP.
1.2 o-hydroxyacetophenone oxidation method
o-hydroxyacetophenone oxidation method is to obtain isophorone IP by reducing o-hydroxyacetophenone through oxidation reaction. The specific process is as follows:
Oxidation reaction: o-hydroxyacetophenone is reacted with trichloroisocyanuric acid, and then potassium permanganate is added for oxidation reaction to generate an oxidation product of o-hydroxyacetophenone.
reductive decomposition: add the oxidation product to sulfuric acid, then add sodium hydroxide, stir the reaction, reductive decomposition to generate isophorone IP. The advantage of this process is that the product obtained is of high purity and no by-products. But the disadvantage is that the process is complex and the cost is high.
2. Preparation method of isophorone IP
2.1 anhydrous triethylamine method
anhydrous triethylamine method is to obtain isophorone IP by refluxing reaction of o-hydroxyacetophenone and isoprene in the presence of anhydrous triethylamine. The specific process is as follows:
Preparation of raw materials: o-hydroxyacetophenone and isoprene are mixed, and reacted in anhydrous triethylamine. The reaction temperature is 50-60 ° C., and the reaction time is about 12 hours. Isophorone IP was obtained.
The advantages of this method are simple process, mild reaction conditions, and no excessive equipment and operations. However, the disadvantage is that the product obtained by this method contains more impurities and has lower purity.
2.2 diazo decarboxylation reaction
diazo decarboxylation reaction is through the diazotization reaction of o-hydroxyacetophenone, and then after decarboxylation reaction, to obtain isophorone IP. The specific process flow of the method is as follows:
Diazotization reaction: o-hydroxyacetophenone is reacted with sodium nitrite to carry out diazotization reaction. The reaction temperature was 0-5°C and the reaction time was 2 hours. The diazotized product is obtained.
decarboxylation reaction: the diazotized product was decarboxylated with sodium bisulfite to obtain isophorone IP. The reaction temperature was 0-5°C and the reaction time was 4 hours. The advantage of
this method is that the product obtained is of high purity and low cost. But the disadvantage is that the process conditions are more harsh, the operation is more difficult.
summary: The above
is a detailed introduction to the production process and preparation method of isophorone IP. Various processes and methods have their advantages and disadvantages, and industrial production needs to choose the most suitable production process according to the specific situation.