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Process for preparing cantharides xanthin

A technology of canthaxanthin and oxidant, which is applied in the fields of oxidative preparation of carbonyl compounds and organic chemistry, can solve problems such as difficulty in initiating oxidation and unstable process, and achieve the effects of stable reaction, simple process operation, and mild reaction conditions

Active Publication Date: 2006-06-28
GUANGZHOU WISDOM BIO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the disadvantages of this method are that it is difficult to initiate oxidation, the process is unstable, and more potassium iodide is used.

Method used

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  • Process for preparing cantharides xanthin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Get 10g beta-carotene and place it in a 500ml reaction kettle, add 250ml dichloromethane, then, get 20g sodium chlorate and dissolve it with 200ml water, then use W(H 2 SO 4 ) = 5% solution to adjust the pH to 3.5, add it to the reaction kettle, control the temperature at 40°C, irradiate the reaction solution with an 800W incandescent lamp, and stir vigorously, react for 4 hours, separate the organic layer, wash with water 3 times, It was then dried with anhydrous sodium sulfate, filtered, and the solution was rotatably evaporated. The residue was washed twice with 200 ml of methanol, and then crystallized with chloroform-methanol to obtain 7.2 g of purple needle-shaped canthaxanthin crystals, with a yield of 70.4%. The obtained canthaxanthin crystal has a melting point of 206-208° C., which is measured according to the method of FAD / WHO, and the product quality meets the food standard stipulated by FAD / WHO.

Embodiment 2

[0022] 10g beta-carotene is placed in 500ml reaction kettle, adds 250ml dichloromethane, then, gets 25g sodium bromate and dissolves with 200ml water, then with W(H 2 SO 4 ) = 5% solution to adjust the pH to 4, add it to the reaction kettle, control the temperature at 35°C, place a 500W mercury lamp on the surface of the reaction liquid to irradiate, and stir vigorously, react for 5 hours, separate the organic layer, and wash with water 3 times , and then dried with anhydrous sodium sulfate, filtered, and the solution was rotary evaporated, the residue was washed twice with 200ml of methanol, and then crystallized with chloroform-methanol to obtain 7.6g of purple needle-shaped canthaxanthin crystals, with a yield of 74.3%. The obtained cantharidin crystals had a melting point of 206-208°C.

Embodiment 3

[0024] Get 10g beta-carotene and place it in a 500ml reaction kettle, add 300ml chloroform, then, get 20g sodium chlorate and dissolve it with 200ml water, then use W(H 2 SO 4 ) = 5% solution to adjust the pH to 3, add it to the reaction kettle, control the temperature at 30 ° C, place a 200W sodium lamp in the reaction solution for irradiation, and stir vigorously, react for 6 hours, separate the organic layer, wash 3 times with water, and then Dry over anhydrous sodium sulfate, filter, and rotary evaporate the solution. The residue is washed twice with 200 ml of methanol, and then crystallized with chloroform-methanol to obtain 6.9 g of purple needle-shaped canthaxanthin crystals, with a yield of 67.5%. The obtained cantharidin crystals had a melting point of 206-208°C.

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Abstract

The invention relates to a manufacture method for cantharis xanthine that dissolving beta-carotene into halogenated hydrocarbon adding oxidizing agent water solution that the ph value is adjusted to 2-5, irradiating under 200-800W lighting to make cantharis xanthine. The invention is easy to operate, stable reaction, mild reaction condition and low cost.

Description

field of invention [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of canthaxanthin. Background technique [0002] Canthaxanthin (or claiming cantharidin) of the present invention is a kind of carotenoid, exists in some mushrooms, crustaceans, fish, algae, egg, blood and liver [Ling Guanting, food additive handbook [M], Beijing, Chemical Industry Press, second edition, 1997,0415-0416], in 1984, FDA / WHO approved canthaxanthin to be included in food additives and formulated quality standards. Cantharidin can be used as a food additive in beverages, ice cream, waffle biscuits, sauces, processed tomato products and processed meat products. Canthaxanthin is added to the feed of poultry such as chickens and ducks, and the egg yolk produces a kind of orange color that consumers like [PAUT J.Recent Progress in Commercial Retinoids and and Carotenoids[J], Pure&ApplChem., 1991, 63(1) 45-48]. [0003] The preparation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/28C07C49/557
Inventor 吴世林陆豫刘学辉
Owner GUANGZHOU WISDOM BIO TECH
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