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Method for preparing canthaxanthin through oxidation

A technology of canthaxanthin and oxidation method, applied in the direction of organic chemistry, etc., can solve problems such as difficulty in causing oxidation, unstable process, etc., and achieve the effects of good stability, stable reaction, and simple process operation

Inactive Publication Date: 2016-07-20
SHANGYU NHU BIOCHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the disadvantage of this method is that it is difficult to initiate oxidation, the process is unstable, more potassium iodide is used, and the excess oxidant needs to be neutralized with sodium thiosulfate, which is extremely difficult for wastewater or solid waste treatment.

Method used

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  • Method for preparing canthaxanthin through oxidation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Take 26.8g (0.05mol) of β-carotene and put it into a 1000ml four-necked flask, add 600ml of dichloromethane and stir to dissolve, then put the four-necked flask into a water bath to heat; add 21.6g (0.2mol) of thiourea peroxide Put it into a 500ml beaker, add 200ml of water, dissolve at room temperature, and transfer it to a 250ml constant pressure dropping funnel after the dissolution is complete. When the temperature in the four-neck flask rises to 30°C, start to add the thiourea peroxide solution dropwise, and the dropping time is controlled at about 1 hour. During the dropping process, the temperature must not exceed 40°C. After the dropping is completed, keep the reaction at 30°C for 8 hours. The organic layer was separated, washed and extracted three times with water, and the organic layer was separated after washing. The organic layer was rotary evaporated, and the solvent was completely removed to obtain 25 g of crude oil. Under HPLC conditions, with AE.LICHROM...

Embodiment 2

[0029] Take 26.8g (0.05mol) of β-carotene and put it into a 1000ml four-necked flask, add 600ml of dichloromethane and stir to dissolve, then put the four-necked flask into a water bath to heat; add 21.6g (0.2mol) of thiourea peroxide Put it into a 500ml beaker, add 200ml of water, dissolve at room temperature, and transfer it to a 250ml constant pressure dropping funnel after the dissolution is complete. When the temperature in the four-neck flask rises to 35°C, start to add thiourea peroxide solution dropwise, and the dropping time is controlled at about 1 hour. During the dropping process, the temperature must not exceed 40°C. After dropping, keep the reaction at 38°C for 16 hours. The organic layer was separated, washed and extracted three times with water, and the organic layer was separated after washing. The organic layer was rotary evaporated, and the solvent was completely removed to obtain 27.3 g of crude oil. Dissolve the crude oil in 300ml of ethanol, heat up to f...

Embodiment 3

[0031] Take 26.8g (0.05mol) of β-carotene and put it into a 1000ml four-necked flask, add 600ml of dichloromethane and stir to dissolve, then put the four-necked flask into a water bath to heat; add 21.6g (0.2mol) of thiourea peroxide Put it into a 500ml beaker, add 200ml of water, dissolve at room temperature, and transfer it to a 250ml constant pressure dropping funnel after the dissolution is complete. When the temperature in the four-neck flask rises to 35°C, start to add thiourea peroxide solution dropwise, and the dropping time is controlled at about 1 hour. During the dropping process, the temperature must not exceed 40°C. After dropping, keep the reaction at 38°C for 16 hours. The organic layer was separated, washed and extracted three times with water, and the organic layer was separated after washing. The organic layer was rotary evaporated, and the solvent was completely removed to obtain 27.1 g of crude oil. Dissolve the crude oil in 300ml of methanol, heat up to ...

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Abstract

The invention discloses a method for preparing canthaxanthin through oxidation.The method includes the steps that beta-carotene serves as the raw material, sulfur oxide urea or urea peroxide serves as an oxidizing agent, an oxidizing reaction is conducted, and the canthaxanthin is obtained.The method has the advantages that operation is simple, the reaction is stable, and the trigger condition is mild; the oxidizing agents including sulfur oxide urea and urea peroxide can be decomposed into H2O2 and elemental oxygen in solvent, O2 is released slowly, the content of active oxygen is high, stability is high, the utility of time is long, no side effect exists, no toxin or public hazard exists, and it is beneficial to achieve industrialized clean production.

Description

technical field [0001] The invention relates to a preparation method of cantharidin, in particular to a method for preparing cantharidin by an oxidation method. Background technique [0002] Canthaxanthin, also known as canthaxanthin, chemical name: β-carotene-4,4’-dione, is a carotenoid. Cantharidin is dark purple crystal or crystalline powder with a melting point of about 210°C (decomposition). It should be stored in a light-shielding container filled with inert gas. Soluble in chloroform (10%), slightly soluble in vegetable oil (0.005%), acetone (0.03%), insoluble in water, ethanol, propylene glycol. The stable commercial product is in the form of a solution in fat or organic solvent, or in the form of a water-dispersible orange to red powder or granules. [0003] The existing preparation methods of canthaxanthin mainly include synthesis method, oxidation method and biological fermentation method etc. Among them, the synthetic method to prepare cantharidin has a long r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C403/24
Inventor 任光明韦念想吕国锋黄国东王力陈晓庆张德胜
Owner SHANGYU NHU BIOCHEM IND
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