Preparation method of isooctyl salicylate

A technology of isooctyl salicylate and methyl salicylate, which is applied in the field of compound preparation, can solve problems such as high reaction temperature and limited economic benefits, and achieve the effects of high purity, improved economic benefits, and low production cost

Active Publication Date: 2012-11-14
江苏普源化工有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is still a small amount of methyl salicylate at the end of this method reaction, and its reason is that sodium methylate can attack the carbocation of salicylic acid parent as a kind of strong nucleophile, causes there to be a reaction bala

Method used

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  • Preparation method of isooctyl salicylate

Examples

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Example Embodiment

[0020] The preparation method of isooctyl salicylate of the present invention includes the following steps:

[0021] In the first step, a 70%-99.9% pure isooctyl alcohol solution is added to the methyl salicylate solution with a purity of 70%-99.9%, and methyl salicylate and isooctyl are added to the methyl salicylate solution. The molar ratio of isooctyl alcohol in the alcohol solution is 1:1 to 1:3, and the mixture is stirred for 1-3 hours to form a homogeneously mixed raw material solution.

[0022] Preferably, in the first step, the molar ratio of methyl salicylate in the methyl salicylate solution to isooctyl alcohol in the isooctyl alcohol solution is 1:2.

[0023] In the second step, a solid inorganic base catalyst is added to the raw material solution prepared in the first step, and the mass of the inorganic base catalyst is 0.2%-1.0% of the mass of the raw material solution to form a reaction solution.

[0024] In the second step, the inorganic base catalyst is sodium hydroxi...

Example Embodiment

[0030] Example 1

[0031] Add 20 mL of 99.9% purity methyl salicylate solution and 40 mL of 99.9% purity isooctanol solution into a 150 mL three-necked flask, and stir for 1 hour. After stirring, a uniformly mixed raw material solution is formed. Add 0.3 g of NaOH to the raw material solution to form a reaction solution; and install a distillation head, a condenser, a tail tube, and a receiving bottle on the three-necked flask. The reaction solution was heated to 150°C, stirred and reacted for 10 hours, the methanol in the receiving flask was recovered, the three-neck flask was cooled to 80°C, the reaction solution was washed twice with hot water at 100°C, and the organic phase was separated and extracted. Use anhydrous Na 2 SO 4 Dry the organic phase. After standing for 8 hours, remove the Na in the organic phase 2 SO 4 . Carry out oil pump vacuum distillation: first use an oil pump to remove the pre-boiler isooctyl alcohol in the organic phase, then heat the container containi...

Example Embodiment

[0037] Example 2:

[0038] Add 40 mL of 70% pure methyl salicylate solution and 80 mL of 85% pure isooctyl alcohol solution to a 250 mL three-necked flask, stir for 3 hours, and stir well to form a uniformly mixed raw material solution. Add 0.6 g of NaOH to the raw material solution to form a reaction solution; and install a distillation head, a condenser, a tail tube, and a receiving bottle on the three-necked flask. The reaction solution was heated to 100°C, stirred and reacted for 4 hours, the methanol in the receiving flask was recovered, the three-neck flask was cooled to 20°C, the reaction solution was washed three times with 50°C hot water, and the organic phase was separated and extracted. Use anhydrous Na 2 SO 4 Dry the organic phase. After standing for 12 hours, remove the Na in the organic phase 2 SO 4 . Carry out oil pump vacuum distillation: first use an oil pump to remove the pre-boiler isooctyl alcohol in the organic phase, and then heat the container containing t...

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Abstract

The invention discloses a preparation method of isooctyl salicylate, which comprises the following steps: 1. adding an isooctyl alcohol solution into a methyl salicylate solution, and stirring for 1-3 hours to form a raw material solution; 2. adding an inorganic alkali catalyst into the raw material solution to form a reaction solution; 3. heating the reaction solution to 100-200 DEG C, stirring to react for 4-10 hours, cooling the reaction solution to 20-80 DEG C, washing the reaction solution with 50-100 DEG C hot water, separating, and extracting an organic phase; and 4. adding anhydrous Na2SO4 into the organic phase to dry the organic phase, standing, removing the Na2SO4 in the organic phase, adding the organic phase into a flask, carrying out vacuum distillation with an oil pump, and collecting the 174-178 DEG C/1.0kPa fraction which is the isooctyl salicylate. The isooctyl salicylate prepared by the preparation method disclosed by the invention has the advantages of high recovery rate, high purity and low preparation cost.

Description

technical field [0001] The present invention relates to a kind of preparation method of compound, specifically, relate to a kind of preparation method of isooctyl salicylate. Background technique [0002] 2-Hydroxy-benzoic acid (2-ethylpentyl) ester (isooctyl salicylate) chemical formula is as follows: [0003] [0004] Isooctyl salicylate (also known as 2-ethylpentyl salicylate) is an important chemical product. It is a colorless to pale yellow transparent liquid with a slightly aromatic smell. It is resistant to UVB (Chinese: outdoor Ultraviolet rays) have absorption and are widely used in perfume, soap, sunscreen cosmetics, and pharmaceutical industries. They can also be used as organic solvents and organic synthesis intermediates. At present, my country mainly relies on imports. [0005] The industrial synthesis of isooctyl salicylate mainly uses salicylic acid as raw material, and concentrated sulfuric acid is used as a catalyst for direct esterification. This method...

Claims

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Application Information

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IPC IPC(8): C07C69/84C07C67/03
Inventor 孙柏旺王燕徐冰左荣林
Owner 江苏普源化工有限公司
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