Preparation method of vitamin E

A vitamin and organic solvent technology, applied in the field of vitamin E preparation, can solve problems such as poor product purity and low yield, and achieve the effects of short reaction time, easy availability of raw materials, and overall cost reduction

Inactive Publication Date: 2012-07-18
ANHUI BBCA FERMENTATION TECH ENG RES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to overcome the defects of low yield and poor product purity of the existing vitamin E pr

Method used

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  • Preparation method of vitamin E

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] At room temperature, put 180g of 2,3,5-trimethylhydroquinone, 180g of zinc chloride, 420mL of toluene, and 20g of 36% hydrochloric acid into a 1L four-neck flask under nitrogen protection, and stir for 20 minutes. The water bath was heated to 40°C, and the nitrogen flow was stopped. Then dropwise add 362g of isophytic alcohol, and control the dropwise addition in about 2 hours. After the isophytic alcohol is added dropwise, add 1.9g of zinc powder under the protection of nitrogen gas, then stop the nitrogen gas flow, maintain the heating temperature at about 40°C, keep warm for 2 hours, then pass nitrogen gas protection to cool, and filter. Add 120mL of water, stir, pour into a separatory funnel and let stand for 20 minutes to separate layers, and remove the water layer. Add 120mL of 1% sodium bicarbonate solution by mass, stir, pour into a separatory funnel and let stand for 20 minutes to separate layers, and remove the water layer. Then add 120mL of pure water, stir...

Embodiment 2

[0025] At room temperature, 180 g of trimethylhydroquinone, 180 g of zinc chloride, 300 mL of benzene, and 15 g of 35% hydrochloric acid by mass were put into a 1L four-neck flask under nitrogen protection, and stirred for 15 minutes. The water bath was heated to 55°C, and the nitrogen flow was stopped. Then dropwise add 340g isophytic alcohol, and control the dropwise addition in about 3 hours. After the isophytic alcohol is added dropwise, add 3.0g of zinc powder under the protection of nitrogen gas, then stop the nitrogen gas flow, maintain the heating temperature at about 55°C, keep warm for 3 hours, then pass nitrogen gas protection to cool, and filter. Add 150mL of water, stir, pour into a separatory funnel and let stand for 25 minutes to separate layers, and remove the water layer. Add 150mL of 1% potassium bicarbonate solution by mass, stir, pour into a separatory funnel and let stand for 25 minutes to separate layers, and remove the water layer. Then add 120mL of pu...

Embodiment 3

[0027] At room temperature, put 180g of 2,3,5-trimethylhydroquinone, 195g of zinc chloride, 480mL of toluene, and 42g of 25% hydrochloric acid into a 1L four-neck flask under nitrogen protection, and stir for 20 minutes. The water bath was heated to 35°C, and the nitrogen flow was stopped. Then dropwise add 380g of isophytic alcohol, and control the dropwise addition in about 3 hours. After the isophytic alcohol is added dropwise, add 1.0g of zinc powder under the protection of nitrogen gas, then stop the nitrogen gas flow, maintain the heating temperature at about 35°C, keep warm for 4.5 hours, and then pass nitrogen gas protection to cool and filter. Add 100mL of water, stir, pour into a separatory funnel and let stand for 20 minutes to separate layers, and remove the water layer. Add 100 mL of 1% potassium bicarbonate solution by mass, stir, pour into a separatory funnel and let stand for 30 minutes to separate layers, and remove the water layer. Then add 120mL of pure wa...

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Abstract

The invention relates to a preparation method of vitamin E. The vitamin E is prepared by reacting 2,3,5-trimethylhydroquinone and isophytol serving as starting raw materials in an organic solvent in the presence of Lewis acid, hydrochloric acid and a metal reducing agent. In the technical scheme of the invention, a small amount of metal reducing agent is added into a reaction system for serving as a protective agent to prevent a generated vitamin E product to be oxidized, so that the purity and yield of a target product are ensured. Moreover, the technical scheme of the invention has the advantages of readily-available raw materials, simple and convenient process, low reaction low consumption and easiness for operating, so that the overall cost is reduced, and the method is suitable for industrial mass production.

Description

technical field [0001] The invention relates to the field of fine chemical synthesis, in particular to a method for preparing vitamin E. Background technique [0002] Vitamin E is the general term for tocopherol compounds. The appearance is golden yellow or light yellow viscous oily liquid with a mild and special smell. It is easily oxidized and turns dark red when exposed to air and light. It can be miscible with acetone, ether or vegetable oil , is almost insoluble in water, and is a fat-soluble antioxidant. Vitamin E is not only a commonly used drug and nutritional health product, but also has many important uses in other fields. Commercial 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. Vitamin E has become the main vitamin variety with a wide range of uses and a large production and sales volume in the international market. Together...

Claims

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Application Information

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IPC IPC(8): C07D311/72
Inventor 李荣杰
Owner ANHUI BBCA FERMENTATION TECH ENG RES
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