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A kind of imidazole ionic liquid and its preparation and application in vitamin e acetate synthesis

A technology of ionic liquids and imidazoles, which is applied in the field of imidazole ionic liquids and their preparation and in the synthesis of vitamin E acetate, which can solve the problems of large environmental pollution, difficult catalyst recovery, and high catalyst prices

Active Publication Date: 2020-10-27
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problems of this process are that the amount of catalyst is high, the recovery of catalyst is difficult, and the environmental pollution is also relatively large.
[0007] In recent years, with the in-depth research on vitamin E, many better catalysts have been developed. For example, researchers from Switzerland's Dessmann recently used rare earth element compounds to replace the traditional zinc chloride and hydrochloric acid system. The effect is better, but The price of rare earth compounds as catalysts is too high, and it is unrealistic to apply them in industrial production

Method used

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  • A kind of imidazole ionic liquid and its preparation and application in vitamin e acetate synthesis
  • A kind of imidazole ionic liquid and its preparation and application in vitamin e acetate synthesis
  • A kind of imidazole ionic liquid and its preparation and application in vitamin e acetate synthesis

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Weigh 55g (0.25mol) of 1-butyl-3-methylimidazole bromide and 34g (0.25mol) of zinc chloride and add them to a reaction flask with a reflux condenser and nitrogen protection, and use an appropriate amount of n-heptane to make Solvent, under constant temperature condition of 105°C, magnetically stirred for 12h. After the reaction was completed, the n-heptane was removed by rotary evaporation under reduced pressure, and the light yellow viscous transparent ionic liquid bromide-1-butyl-3-methylimidazolium zinc chloride salt ionic liquid was obtained after vacuum drying, with a yield of 96%.

[0033] Product characterization: 1 H NMR (500MHz, DMSO): δ0.80(t, 3H, J=7.3Hz), 1.19(m, 2H), 1.70(m, 2H), 3.80(s, 3H), 4.10(t, 2H, J =7.2Hz),7.55(s,1H),7.61(s,1H),8.92(s,1H).

Embodiment 2

[0035] Weigh 55g (0.25mol) of 1-butyl-3-methylimidazole bromide and 56g (0.25mol) of zinc bromide into a reaction flask equipped with a reflux condenser and nitrogen protection, and use an appropriate amount of n-heptane to make Solvent, under constant temperature condition of 105°C, magnetically stirred for 12h. After the reaction was completed, the n-heptane was removed by rotary evaporation under reduced pressure, and the light yellow viscous transparent ionic liquid bromide-1-butyl-3-methylimidazolium zinc bromide ionic liquid was obtained after vacuum drying with a yield of 98%.

[0036] Product characterization: 1 H NMR (500MHz, DMSO): δ0.80(t, 3H, J=7.3Hz), 1.19(m, 2H), 1.70(m, 2H), 3.80(s, 3H), 4.10(t, 2H, J =7.2Hz),7.55(s,1H),7.61(s,1H),8.92(s,1H).

Embodiment 3

[0038] Weigh 2.5g bromide-1-butyl-3-methylimidazolium zinc chloride salt ionic liquid and 10.00g 2,3,5-trimethylhydroquinone diacetate into the reaction bottle, then add 45mL petroleum ether As a solvent, an oil bath was used to heat the temperature of the reaction liquid to 70° C., and with magnetic stirring, 12.55 g of isophytic alcohol was slowly added dropwise with a constant pressure funnel, and the reaction time was controlled at 4 hours. After the reaction, the reaction solution was left to stand, and the catalyst and vitamin E were separated, then 4.32g of acetic anhydride was weighed and added to the product, and the oil bath was 120°C, and the reaction was carried out for 3 hours to obtain the final product vitamin E acetate with a yield of 80%. , the selectivity is 88%, and the catalyst separated by cooling and standing can be recycled.

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Abstract

The invention discloses an imidazole ionic liquid, a preparation method thereof, and an application thereof in the synthesis of vitamin E acetate. The structure of the imidazole ionic liquid is represented by formula (I) shown in the description, and Y in the formula (I) is ZnCl2Br<-> or ZnBr<3><->. The catalyst has the advantages of cheapness, easiness in obtaining, and stable performances, and has the advantages of good catalytic activity, simple reaction process, mild reaction conditions, high conversion rate and selectivity and no pollution when used in catalytically synthesizing the reaction of vitamin E.

Description

[0001] (1) Technical field [0002] The invention relates to an imidazole ionic liquid, its preparation and its application in the synthesis of vitamin E acetate. [0003] (2) Background technology [0004] Vitamin E (Vitamin E), molecular formula C 29 h 50 o 2 , with a relative molecular mass of 430.71, is a fat-soluble vitamin. Vitamin E acetate is V E One of the ester derivatives, it has the functions of anti-oxidation, moisturizing, enhancing the body's immunity, eliminating free radicals in the body, and preventing cancer. Therefore, it has been widely used in the pharmaceutical and cosmetic industries, such as treating various inflammations. Most high-end shampoos, moisturizing creams, and facial cleansers contain vitamin E acetate. Vitamin E acetate is also widely used in the food and feed industry. [0005] Ionic liquid, also known as room or ambient temperature ionic. In recent years, ionic liquids have received great attention as a new environmentally friendly ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/58B01J31/02C07D311/72
CPCB01J31/0284B01J2231/49C07D233/58C07D311/72
Inventor 郭红云潘鹏金春晖
Owner ZHEJIANG UNIV OF TECH
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