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A kind of synthetic preparation method of wintergreen oil

A technology for wintergreen oil and synthesis reaction, which is applied in the preparation of organic compounds, preparation of carboxylic acid esters, chemical instruments and methods, etc., can solve the problems of complex catalyst preparation process, complex post-reaction treatment, complex synthesis reaction, etc., and shorten the production time. The effect of cycle, easy purification, and simple reaction process

Active Publication Date: 2022-02-18
江西省隆南药化有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method overcomes some defects of the traditional concentrated sulfuric acid catalytic method, it still has the disadvantages of using p-toluenesulfonic acid as a catalyst, which is expensive and difficult to recycle; Preparation process of methyl salicylate", the preparation process adopts sol-gel technology to prepare TiO2 composite photocatalyst, instead of traditional concentrated sulfuric acid catalyst
Although this process overcomes some defects of the traditional concentrated sulfuric acid catalysis method, there are disadvantages such as the use of TiO2 composite photocatalyst, the preparation process of the catalyst is complicated, the whole synthesis reaction is complicated, the practicability is poor, and the follow-up treatment of the reaction is complicated; another example: Publication No. The patent name of CN105622403A is "a method for the synthesis and preparation of high-quality methyl salicylate". The synthesis method uses a new catalyst to replace the original concentrated sulfuric acid catalyst. and additives, wherein the base material is silicon dioxide, diatomaceous earth and aluminum oxide, and the polysaccharide is one or more of polyacetylglucosamine, galactose and polyfructose, and the sulfide It is one or both of potassium hydrogen sulfate and copper sulfate, and the auxiliary agent is one or both of polyvinyl alcohol and polysorbate
Although this synthesis method overcomes some defects of the traditional concentrated sulfuric acid catalytic method, there are still shortcomings such as complex preparation process of the catalyst, poor practicability, and complicated post-reaction treatment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: Catalyst as methylene carboxylate - small test preparation of winter boiled oil

[0023] According to the ratio of molar ratio 2: 1: 0.2, 128.16 g of methanol, 276.24 g of salicylic acid, 24.02 g of formate, sequentially put into high pressure reactor, control the reaction temperature 150 ° C, pressure 0.9 MPa, in agitation The reaction was at 6 h. After the reaction was completed, the reaction solution was transferred to the normal temperature, and the 25 cm filler column (the Bauer ring of the ceramic material) was crude, and the methanol fraction of 30-66 ° C was collected. After the collection is completed, the vacuum pressure is controlled at -0.09 ~ -0.10 MPa, and the fraction of 75-80 ° C is collected until there is no liquid steamed. 298.45 g of finished winter oil was obtained, with a purity of 99.6%, and the conversion rate was 97.78%.

Embodiment 2

[0024] Example 2: Catalyst as a methyl acetate - small test prepared for winter oil:

[0025] According to the ratio of molar ratio 2: 1: 0.2, 128.16 g of methanol, 276.24 g of salicylic acid, methyl acetate 29.63 g, sequentially put into the high pressure reactor, control the reaction temperature at 150 ° C, pressure at 0.9 MPa, The reaction was reacted for 6 h. After the reaction was completed, the reaction solution was transferred to the three-necked flask, and the 25 cm filler column (in the filler of the ceramic material) was crude, and the fraction of 50-66 ° C was collected. After the collection is completed, the vacuum pressure is controlled at -0.09 ~ -0.10MPa, and the fraction of 75-80 ° C is collected, and until there is no liquid steamed. 272.01 g of finished winter oil was obtained, and the product purity was 99.6%, the conversion rate was 89.12%.

Embodiment 3

[0026] Example 3: Catalyst as methyl butyrorate - Try prepared winter oil:

[0027] According to the ratio of molar ratio 2: 1: 0.2, 128.16 g of methyl alcohol was accurately weighed, 276.24 g of salicylic acid was 20.85 g of butyrate, and the high pressure reactor was sequentially put into the high pressure reactor, the reaction temperature was 150 ° C, the pressure was 0.9 MPa, The reaction was reacted at a stirred state. After the reaction was completed, the reaction mixture was transferred to the normal temperature, and the 25 cm filler column (the Bauer ring of the glass material was carried out in normal pressure, and the fraction of 50-66 ° C was collected. After the collection is completed, the vacuum pressure is controlled at -0.09 ~ -0.10 MPa, and the fraction of 75-80 ° C is collected until there is no liquid steamed. 263.52 g of finished winter oil was obtained, and the purity of the product was 99.5%, the conversion rate was 86.25%.

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Abstract

The invention relates to the field of chemical synthesis, and specifically discloses a synthetic preparation method of wintergreen oil. The method comprises the following steps: (1) according to the molar ratio of 2-3:1:0.1-0.3, methanol, salicylic acid and methyl carboxylate are sequentially put into the reactor; (2) under the condition of heating and pressurizing , a synthesis reaction occurs to obtain a mixed solution A containing wintergreen oil; (3) distilling and separating the mixed solution A to obtain wintergreen oil. This method not only overcomes the defects of the traditional concentrated sulfuric acid catalytic method, but also uses methyl carboxylate as the catalyst, which has the advantages of easy access to raw materials, simple reaction process, simple distillation to remove the catalyst, and simple follow-up treatment. The prepared wintergreen oil has beneficial effects such as high product purity and high conversion rate.

Description

Technical field [0001] The present invention belongs to the field of chemical synthesis, and in particular to a synthetic preparation method of winter green oil. Background technique [0002] Holly oil has a winter blue aroma, which is also known as methyl salicylate, which is widely existed in nature, and is the main component of deer hoist and small medicinal oil. It is now widely used in fine product chemicals, preservatives, fixtures, also used as spices such as beverages, food, toothpaste, cosmetics, etc., and for producing painkillers, pesticides, rubber, inks and Fiber-assisted agents, while their ability to inflammation, analgesia, bactericidal effects, and transdermal skin are widely used in the pharmaceutical industry. [0003] Traditional wintering oil synthesis methods are mainly esterification. The method was carried out under a concentrated sulfuric acid catalysis with salicylic acid and methanol. Although concentrated sulfuric acid as a catalyst has a high catalyti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/84
CPCC07C67/08
Inventor 万贵生刘遗松赖神风钟庆瑜梁毅
Owner 江西省隆南药化有限公司
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