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Method for preparing vitamin A and vitamin A ester

A vitamin and production method technology, which is applied in the fields of dehydrogenation preparation, carbon-based compound preparation, chemical instruments and methods, etc., can solve problems such as unfavorable industrial production and long steps, and achieves few reaction steps, mild reaction conditions, and yield. high effect

Active Publication Date: 2020-04-03
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This route has long steps and uses a variety of special reagents, which is not conducive to industrial production

Method used

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  • Method for preparing vitamin A and vitamin A ester
  • Method for preparing vitamin A and vitamin A ester
  • Method for preparing vitamin A and vitamin A ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Add 1170g of farnesol, 2L of DMF, 12g of TEMPO, and 12g of cuprous chloride into the reactor, stir, and raise the temperature to 50°C. Oxygen was continuously introduced, and the reaction was maintained at 50°C for 0.5h. After the reaction was completed, the solvent was removed and distillation under reduced pressure was carried out to obtain 1066 g of farnesal with a content of 98% and a yield of 95%. 1H NMR (300MHz, CDCl 3 ) characterization results are: δ=9.78(s,1H),5.75(m,1H),5.26(m,1H),5.16(m,1H),2.03(m,8H),1.86(s,3H),1.80 (s,6H),1.75(s,3H).

[0063] Add 1000g of farnesal, 1226g of DDQ, 4L of toluene into the reactor, and stir. Raise the temperature to 50°C and react for 0.5h. After the reaction was finished, the solvent was removed, and the dehydrofarnesal was distilled under reduced pressure to obtain 940 g of dehydrofarnesal with a content of 98% and a yield of 95%. 1 H NMR (300MHz, CDCl 3 ) characterization results are: δ=9.76(s,1H),6.53(m,2H),6.40(m,1H),...

Embodiment 2

[0068] Add 1170g of farnesol, 2L of DMF, 2.3g of 4-hydroxy-TEMPO, and 2.3g of cuprous chloride into the reactor, stir and keep at 30°C. Continue to feed air, and keep at 30°C for 2h. After the reaction was completed, the solvent was removed and distillation under reduced pressure was carried out to obtain 1090 g of farnesal with a content of 98% and a yield of 97%.

[0069] Add 1000g farnesal, 1162g chloranil, 4L tetrahydrofuran into the reactor, and stir. Keep at 30°C and react for 2h. After the reaction was completed, the solvent was removed, and the dehydrofarnesal was distilled under reduced pressure to obtain 931 g of dehydrofarnesal with a content of 98% and a yield of 94%.

[0070] Add 450g of phosphoric acid, 900g of dehydrofarnesal, and 1800g of toluene into the reactor, and stir. Raise the temperature to 50°C and react for 3h. After the reaction was completed, the temperature was lowered to room temperature, and the phases were separated. After removing the solv...

Embodiment 3

[0074] Add 1170g of farnesol, 2L of DMF, 1.2g of 4-methoxy-TEMPO, and 1.2g of cuprous chloride into the reactor, stir and keep at 40°C. Oxygen was continuously introduced, and the reaction was maintained at 40° C. for 1 h. After the reaction was completed, the solvent was removed and distillation under reduced pressure was carried out to obtain 1090 g of farnesal with a content of 98% and a yield of 97%.

[0075] Add 1000g farnesal, 1070g DDQ, 4L ethyl acetate into the reactor, and stir. Keep at 40°C and react for 1h. After the reaction was completed, the solvent was removed, and the dehydrofarnesal was distilled under reduced pressure to obtain 922g of dehydrofarnesal with a content of 98% and a yield of 93%.

[0076] Add 900g of trifluoromethanesulfonic acid, 900g of dehydrofarnesal, and 1800g of dichloromethane into the reactor, stir, and heat at 40°C for 3h. After the reaction was completed, the temperature was lowered to room temperature, and the phases were separated....

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Abstract

The invention provides a novel method for preparing vitamin A and vitamin A ester by taking farnesol as a raw material. The method comprises the following steps: carrying out oxidation reaction on farnesol and oxygen under the action of a catalyst and a cocatalyst to generate farnesal; carrying out dehydrogenation reaction on farnesal to generate dehydrofarnesal; carrying out cyclization reactionon the dehydrofarnesal under the catalysis of acid to generate a cyclized intermediate; carrying out a reaction on the cyclized intermediate with chloroisopentenol to generate vitamin A; carrying outan esterification reaction on vitamin A to generate vitamin A ester. The method avoids the defects of an existing process, and the process line is economical and effective.

Description

technical field [0001] The invention belongs to the field of fine chemical synthesis, and in particular relates to a preparation method of vitamin A and vitamin A ester. Background technique [0002] Vitamin A acetate is an important class of nutritional chemicals, which can promote the growth and development of the human body, and can enhance the resistance to diseases. At the same time, vitamin A acetate is also an important feed additive, which has various physiological functions such as promoting the synthesis of animal immunoglobulins, promoting growth and reproduction. [0003] At present, there are mainly two technical routes for the synthesis of vitamin A esters in industry. [0004] One is the C14+C6 route [0005] [0006] The other is the C15+C5 route [0007] [0008] The two routes have their own defects. The C14+C6 route requires more than 50 kinds of raw materials, the reaction steps are long, the fixed investment is large, and it is a series reaction...

Claims

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Application Information

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IPC IPC(8): C07C403/08C07C403/12C07C403/14C07C45/00C07C45/38C07C47/21
CPCC07C403/08C07C403/12C07C403/14C07C45/002C07C45/38C07C2601/16C07C47/21
Inventor 吕英东王展张涛黎源
Owner WANHUA CHEM GRP CO LTD
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