Synthetic method of homosalate

A kind of technology of homosalate and synthesis method, applied in the synthesis field of ultraviolet absorber homosalate, to achieve the effect of simple operation

Inactive Publication Date: 2016-05-04
NANJING NONGKANG BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to overcome the difficulties and deficiencies in the prior art, the inventors tried to synthesize homosalate through transesterification under acid or alkali catalysis with lower alkyl salicylate and 3,3,5-trimethylcyclohexanol, The lower alkyl refers to C1-C6 alkyl, such as methyl, ethyl, propyl, isopropyl, etc.

Method used

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  • Synthetic method of homosalate
  • Synthetic method of homosalate

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Add 10.0g of methyl salicylate and 14.0g of 3,3,5-trimethylcyclohexanol to a 250ml three-necked flask, mix well, add 5.0g of potassium carbonate, increase the temperature to 120-130℃ and react for 10h, monitor the water by gas chromatography The conversion rate of methyl salicylate was 85.6%. Under reduced pressure distillation, 12.2 g of colorless and transparent humosalate was obtained, the yield was 70.8%, and the GC purity was greater than 99%.

Embodiment 2

[0024] Add 10.0g of methyl salicylate, 23.3g of 3,3,5-trimethylcyclohexanol, 0.50g of potassium carbonate, and 0.1g of tetrabutylammonium bromide into a 250ml three-necked flask. The temperature is raised to 180℃ and reacted for 13h. The conversion rate of methyl salicylate in the reaction system detected by chromatography was 97.2%. It was changed to a vacuum distillation device, and the front fraction was recovered for application to obtain 13.98 g of colorless and transparent humosalate with a yield of 81.1% and a GC purity of greater than 99%.

Embodiment 3

[0026] Add 10.0g of methyl salicylate, 18.7g of 3,3,5-trimethylcyclohexanol, 0.20g of sodium hydroxide, and 0.1g of potassium salicylate to a 250ml three-necked flask. The temperature is raised to 160℃ and the reaction is 8h. Gas chromatography Monitoring the conversion rate of methyl salicylate was 94.8%.

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Abstract

The invention provides a method for synthesizing homosalate through an ester exchange reaction of methyl salicylate or ethyl salicylate and 3,3,5-trimethylcyclohexanol under the catalysis of an alkali. The method has the advantages of simple operation, high conversion rate, economy, environmental protection, and suitableness for industrial production.

Description

Technical field [0001] The invention relates to a method for synthesizing the ultraviolet absorber humosalate. technical background [0002] The ultraviolet rays contained in sunlight are divided into long-wave ultraviolet (UVA) from 320nm-400nm, medium-wavelength ultraviolet (UVB) from 280nm-320nm, and short-wave ultraviolet (UVC) from 200nm-280nm. Ultraviolet rays below 280mn are absorbed by the ozone layer and cannot reach the ground. The ultraviolet rays reaching the ground will have various effects on people's skin. Among them, UVB can cause erythema or water scars on the skin, promote the formation of melanin, cause skin pigmentation, and cause brown The formation of spots. It was previously believed that UVA would not have a major impact on the skin, but it has been proven through electron microscopy or histochemical methods that excessive UVA irradiation will have a certain impact on the skin. UVA segment ultraviolet light is different from UVB, and its energy can be It...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/84C07C67/03
Inventor 陈华明王节鹏马子腾赵坚冯高亮
Owner NANJING NONGKANG BIOTECH CO LTD
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