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Method for synthesizing and preparing high-quality methyl salicylate

A methyl salicylate, high-quality technology, applied in the field of synthesis and preparation of high-quality methyl salicylate, can solve the problem of low purity of methyl salicylate products, long synthesis time of methyl salicylate, unfavorable industrial production etc. to achieve the effects of easy operation, low toxicity and reduced reaction time

Inactive Publication Date: 2016-06-01
ZHENJIANG GAOPENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In existing preparation technology, mostly adopt concentrated sulfuric acid as its acid catalyst, carry out methyl salicylate synthesis, under this kind of method, the synthesis time of methyl salicylate is obviously longer, and the purity of methyl salicylate product Low cost, high cost, and high toxicity during processing and synthesis, which is not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A kind of synthetic preparation method of high-quality methyl salicylate, it is characterized in that, preparation method is as follows:

[0039] (1) Take salicylic acid, methanol and a new catalyst, the weight ratio of salicylic acid, methanol and catalyst is 1:2.6:0.4, put all the salicylic acid and methanol into the mixing tank, stir slowly for 30 minutes, and conduct a water bath Heating, the heating temperature is controlled at 25°C, and the stirring speed is controlled at 660r / min;

[0040] (2) Install a reflux condensing device on the mixing tank, increase the temperature of the water bath to 85°C, and slowly add a new catalyst, react for 3.4 hours, and evaporate excess methanol at the same time;

[0041] (3) Let the remaining liquid in the mixing tank stand to cool, then put it into the liquid separation tank and let it stand for stratification, separate the water layer, and take its organic layer;

[0042] (4) The organic layer was washed successively with wat...

Embodiment 2

[0057] The synthetic preparation method of above-mentioned a kind of high-quality methyl salicylate, wherein, described novel catalyst is prepared from by the raw material component of following weight part:

[0058] 144 parts of base material,

[0059] 34 parts of polysaccharides,

[0060] 2.6 parts of sulfide,

[0061] 9 parts of talcum powder,

[0062] 13 parts of auxiliary agent;

[0063] The preparation method of described novel catalyst is as follows:

[0064] (1) Take base material and sulfide by weight, base material is slowly dropped into ethanol, the volume ratio of ethanol and base material is 8.1:1, throwing into process is accompanied by stirring, stirring time is controlled at 39 minutes, drops into sulfide, And continue to stir for 9 minutes, then let it stand for 2.2 hours, after the acid reaction is completed, pour out the ethanol to obtain the modified base material A;

[0065] (2) Continuously pour distilled water into the modified base material A in step...

Embodiment 3

[0070] The synthetic preparation method of above-mentioned a kind of high-quality methyl salicylate, wherein, described novel catalyst is prepared from by the raw material component of following weight part:

[0071] 143 parts of base material,

[0072] 37 parts of polysaccharides,

[0073] 2.7 parts of sulfide,

[0074] 11 parts of talcum powder,

[0075] 13 parts of auxiliary agent;

[0076] The preparation method of described novel catalyst is as follows:

[0077] (1) Take the base material and the sulfide by weight, slowly drop the base material into ethanol, the volume ratio of ethanol and the base material is 9:1, the input process is accompanied by stirring, the stirring time is controlled at 42 minutes, drop into the sulfide, And continue to stir for 10 minutes, then let it stand for 2.4 hours, after the acid reaction is completed, pour out the ethanol to obtain the modified base material A;

[0078] (2) Continuously pour distilled water into the modified base mat...

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Abstract

The invention discloses a method for synthesizing and preparing high-quality methyl salicylate. An original concentrated-sulfuric-acid catalyst is replaced with a new catalyst. The new catalyst is prepared from base materials, polysaccharide, sulfide, talcum powder and addition agent, wherein base materials are prepared in the mode that silicon dioxide, kieselguhr and aluminum oxide are stirred and mixed; polysaccharide is one or more of poly-N-acetylglucosamine, galactose and polyfructosan; sulfide is one or two of potassium hydrogen sulfate and copper sulfate; addition agent is one or two of polyving akohol and polysorbitol. The new catalyst is stable in quality, even in concentration, steady in preparing-process operation, low in preparing cost, small in toxicity, good in repeatability, easy to operate and suitable for industrial mass production; meanwhile, the method replaces the traditional methyl salicylate synthesizing and preparing method with concentrated sulfuric acid as the catalyst, and the catalytic effect is obvious; meanwhile, the synthetic speed of the methyl salicylate is increased, and reaction time is shortened.

Description

technical field [0001] The invention relates to a method for synthesizing and preparing high-quality methyl salicylate, belonging to the technical field of chemical production. Background technique [0002] Methyl salicylate is a medicine used as a redness agent for external use. It is used clinically to promote local blood circulation. External use or local rubbing can reflectively affect the skin, muscles, nerves and joints of the corresponding parts, and reduce swelling. , anti-inflammatory and analgesic effects, also has antipruritic effect. For sprains, bruises, low back pain, muscle pain, neuralgia, itching. At the same time, it is an important fine chemical intermediate, which is widely used in the fields of medicine, pesticide, spices, fuel, and synthetic additives. [0003] In existing preparation technology, mostly adopt concentrated sulfuric acid as its acid catalyst, carry out methyl salicylate synthesis, under this kind of method, the synthesis time of methyl ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/84B01J31/26B01J31/28
CPCC07C67/08B01J31/26B01J31/28B01J2231/49
Inventor 王成栋王成慧
Owner ZHENJIANG GAOPENG PHARMA
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