A kind of preparation method of vitamin E

A vitamin and catalyst technology is applied in the field of vitamin E preparation to achieve the effects of reducing waste water, good reaction selectivity and high reaction yield

Active Publication Date: 2020-11-06
ZHEJIANG NHU PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the process requires supercritical carbon dioxide as a solvent to achieve high concentration and yield, and there is still room for improvement in the repeatability of ionic liquids.

Method used

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  • A kind of preparation method of vitamin E
  • A kind of preparation method of vitamin E
  • A kind of preparation method of vitamin E

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] In the reaction vessel, add 91.31g (0.6mol) trimethylhydroquinone and 14.87g 3-sulfonic acid propyltrimethylamine chloride zincate [HO 3 S-(CH 2 ) 3 -NMe 3 ][Cl 2ZnCl 2 ], stirred, heated to 99°C under the protection of nitrogen, and slowly added dropwise 177.92g (0.6mol) of isophytic alcohol for 45 minutes. After the reaction is finished, let it stand for cooling, then take the upper and lower layer liquids to recover the solvent under reduced pressure, and obtain the product and the catalyst respectively.

[0035] The product is sampled, and the sample method refers to GB / T 9454-2008, gas chromatography, and the condensation reaction yield is 96.5%.

Embodiment 2

[0037] Add successively 91.31g (0.6mol) trimethylhydroquinone and 14.87g 3-sulfonic acid propyltrimethylamine chloride zincate [HO 3 S-(CH 2 ) 3 -NMe 3 ][Cl 2ZnCl 2 ], stirred, heated to 40° C. under the protection of argon, slowly added dropwise 177.92 g (0.6 mol) of isophytic alcohol for 1 hour, and kept the reaction for 3 hours after the dropwise addition was completed. After the reaction is finished, let it stand for cooling, then take the upper and lower layer liquids to recover the solvent under reduced pressure, and obtain the product and the catalyst respectively.

[0038] The product is sampled, and the sample method refers to GB / T 9454-2008, gas chromatography, and the condensation reaction yield is 92.0%.

Embodiment 3

[0040] Add successively 91.31g (0.6mol) of trimethylhydroquinone and 14.87g of 3-sulfonic acid propyltrimethylamine dissolved in 530ml of heptane / ethylene carbonate (5:4v / v) mixed solvent in the reaction vessel Chlorozincate [HO 3 S-(CH 2 ) 3 -NMe 3 ][Cl 2ZnCl 2 ], stirred, heated to 140° C. under the protection of helium, and added dropwise 177.92 g (0.6 mol) of isophytic alcohol for 20 minutes. After the dropwise addition, the mixture was incubated for 40 minutes. After the reaction is finished, let it stand for cooling, then take the upper and lower layer liquids to recover the solvent under reduced pressure, and obtain the product and the catalyst respectively.

[0041]The product is sampled, and the sample method refers to GB / T 9454-2008, gas chromatography, and the condensation reaction yield is 92.3%.

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PUM

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Abstract

The invention discloses a preparation method of vitamin E. Vitamin E is prepared from trimethylhydroquinone and isophytol by condensation, wherein the condensation is performed in the presence of a Bronsted-Lewis ionic liquid catalyst, and structures of the Bronsted-Lewis ionic liquid catalyst are shown as formulae (A), (B) and (C) in the description. The preparation method has the advantages thatequipment is little corroded, little wastewater is produced, the catalyst is recyclable and easy to separate and losses little, the reaction selectivity is good, the yield is high and the like.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of vitamin E. Background technique [0002] Vitamin E is the general term for tocopherol compounds. It is a golden or light yellow viscous oily liquid with a mild and special smell. Vitamin E is miscible with acetone, ether or vegetable oil, almost insoluble in water, and is a fat-soluble antioxidant. Vitamin E can be divided into two categories: natural vitamin E and synthetic vitamin E. At present, synthetic vitamin E accounts for more than 80% of the global total commodity volume. [0003] In industrial production, vitamin E is generally synthesized by condensation of 2,3,5-trimethylhydroquinone and isophytic alcohol. Traditional processes usually use Lewis acid or protonic acid as the catalyst for the condensation reaction. However, the traditional process will cause equipment corrosion and increase equipment costs. Second, waste...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/72
CPCC07D311/72Y02P20/584
Inventor 乔胜超曾庆宇田金金管敏虾谭均华王立坚傅一苇
Owner ZHEJIANG NHU PHARMA
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