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A kind of preparation method of high-purity cantharidin

A technology of canthaxanthin and carotene, applied in the direction of organic chemistry, can solve the problems of difficulty in accurately grasping the degree of oxidation, low yield, and difficult wastewater treatment, so as to prevent violent reactions from generating by-products, increase yield, and inhibit peroxides The effect of by-products

Active Publication Date: 2020-09-15
安徽工大化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the disadvantages are: the halogen salt used is prone to explosion, and the wastewater treatment in the reaction process is difficult, etc.
However, the two oxidants still make the reaction proceed in two phases, and it is difficult to fully contact the raw materials, oxidants and catalysts, resulting in more difficult reactions and lower yields
[0007] And what above-mentioned method all used is strong oxidizing agent, is difficult to accurately grasp oxidation degree, and peroxidation phenomenon easily takes place, in addition, the purity of the target product canthaxanthin that above-mentioned method obtains is lower

Method used

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  • A kind of preparation method of high-purity cantharidin
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Experimental program
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Effect test

Embodiment 1

[0036] Put 26.84g (0.05mol) of β-carotene and 100ml of dichloromethane in a 500ml three-necked flask, stir and dissolve, then add 1.36ml of 2wt% hydrogen peroxide and 1.66ml of hydrogen peroxide dropwise at a rate of 2 drops / s to the solution. g KI aqueous solution, and then slowly add 32.44 g (0.2 mol) m-chloroperoxybenzoic acid to the reaction system at 25° C., and react for 7 hours to obtain cantharidin produced by oxidation of β-carotene. Detected with an ultraviolet spectrophotometer, the yield of the product cantharidin was calculated to be 81.1%.

[0037] Purification process:

[0038] Add 0.5g antioxidant to the mixture solution containing target product canthaxanthin, described antioxidant is to contain tert-butylphenol antioxidant, wash twice with 5wt% sodium thiosulfate solution, then wash once with deionized water, then The solvent was removed by rotary evaporation to obtain the crude product. The resulting crude product was heated to 60°C in an ethanol solution,...

Embodiment 2

[0040] Put 26.84g (0.05mol) of β-carotene and 100ml of dichloromethane in a 500ml three-necked flask, stir and dissolve, then add 1.36ml of 2wt% hydrogen peroxide and 1.66ml of hydrogen peroxide dropwise at a rate of 2 drops / s to the solution. g KI solution, and then slowly add 32.44 g (0.2 mol) m-chloroperoxybenzoic acid at 35° C., and react for 4 hours to obtain canthaxanthin obtained by oxidation of β-carotene. Detected with an ultraviolet spectrophotometer, the calculated yield of the product cantharidin was 86.8%.

[0041] Purification process:

[0042] Add 0.5 g antioxidant to the mixture solution containing the target product canthaxanthin, wash the obtained solution twice with 5 wt % sodium thiosulfate solution, and wash once with deionized water, then spin evaporate to remove the solvent to obtain the crude product. The obtained crude product was heated to 80° C. in ethanol solution, refluxed for 10 h, and cooled for recrystallization. The solid obtained by recrysta...

Embodiment 3

[0044]Put 26.84g (0.05mol) of β-carotene and 100ml of dichloromethane in a 500ml three-necked flask, stir and dissolve, then add 1.36ml of 2wt% hydrogen peroxide and 1.66ml of hydrogen peroxide dropwise at a rate of 2 drops / s to the solution. g KI solution, then slowly add 32.44 g (0.2 mol) m-chloroperoxybenzoic acid at 30° C., and react for 5 hours to obtain canthaxanthin obtained by oxidation of β-carotene. Detected with an ultraviolet spectrophotometer, the calculated yield of the product cantharidin was 80.6%.

[0045] Purification process:

[0046] Add 0.5 g antioxidant to the mixture solution containing the target product canthaxanthin, wash the obtained solution twice with 5 wt % sodium thiosulfate solution, and wash once with deionized water, then spin evaporate to remove the solvent to obtain the crude product. The obtained crude product was heated to 90° C. in ethanol solution, refluxed for 11 h, and cooled for recrystallization. The recrystallized solid was put in...

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Abstract

The invention discloses a preparation method of high-purity canthaxanthin, and belongs to the technical field of preparation of compounds. The method comprises the following steps: dissolving beta-carotene into an organic solvent, slowly adding excessive 3-Chloroperbenzoic acid serving as an oxidant into solution capable of generating a catalyst, oxidizing the beta-caroteneinto canthaxanthin in anormal temperature condition, performing recrystallization and a hydrothermal reaction for purification, so as to obtain the canthaxanthin with higher purity finally. As the 3-Chloroperbenzoic acid serves as the oxidant and is relatively weak in oxidability, the mild oxidizing reaction can be ensured, and the generation of peroxide by-products can be inhibited fundamentally, so that the purity ofthe product canthaxanthin is improved.

Description

technical field [0001] The invention relates to the technical field of preparation of cantharidin, in particular to a preparation method of high-purity cantharidin. Background technique [0002] Canthaxanthin is an important carotenoid that widely exists in organisms in nature. Because of its good coloring effect and high stability, it is often used as a colorant in food, feed, cosmetics, etc. At the same time, cantharidin is also widely used in the medical field because of its physiological functions. Cantharidin is similar to VE, astaxanthin, β-carotene, etc. in quenching free radicals, which can improve immunity, delay aging, prevent Diseases of old age even have some anti-cancer benefits. The methods of obtaining anthrax mainly include natural raw material extraction, biological fermentation production and chemical synthesis production. Since the content of canthaxanthin in various species is very small, it cannot be mass-produced by artificial extraction; and it is ve...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C403/24
CPCC07C403/24C07C2601/16
Inventor 宋丰发刘艳红许立信张仲谋万超
Owner 安徽工大化工科技有限公司