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Preparation method of campestanol

A technology of campestanol and oleostanol, which is applied in the fields of steroidal compounds and organic chemistry, and achieves the effects of simple process, low cost and efficient synthesis route

Active Publication Date: 2014-04-09
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Campesterol or / and brassicasterol can be obtained by hydrogenation of pure campesterol or / and brassicasterol, but the content of campesterol and brassicasterol in nature is extremely low, and it is difficult to obtain pure campesterol or brassicasterol by separation; at present There is no pure campesterol or brassicasterol, nor is there any pure campesterol on the market

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take 20 g of ergosterol with a content of 95% and dissolve it in 200 mL of n-propanol. After fully stirring, add a hydrogenation reactor; 0.1 g of palladium-carbon catalyst with a palladium content of 10% is added in 5 mL of n-propanol. Add to the hydrogenation reactor after fully stirring; connect the gas pipeline, close the intake valve, pump out the air in the reactor, fill it with hydrogen, and repeat five times. Adjust the hydrogen pressure in the reactor to be 1.5 MPa and the stirring speed to be 200 rpm, and control the temperature in the reactor to be 80 o C, reacted for 9 h.

[0022] After the reaction, the reaction solution was taken out, the catalyst was removed by vacuum filtration, and the organic solvent was removed by rotary evaporation to obtain campestanol. The purity of campestanol was 96.6% by liquid chromatography analysis.

Embodiment 2

[0024] Weigh 10 g of ergosterol with a content of 96% and dissolve it in 400 mL of butyl acetate. After fully stirring, add the hydrogenation reactor; Reactor; connect the gas pipeline, close the intake valve, pump out the air in the reactor, fill it with hydrogen, and repeat five times. Adjust the hydrogen pressure in the reactor to 0.2 MPa and the stirring speed to 600 rpm, and control the temperature in the reactor to 20 o C, reacted for 3 h.

[0025] After the reaction, the reaction solution was taken out, the catalyst was removed by vacuum filtration, and the organic solvent was removed by rotary evaporation to obtain campestanol. The purity of campestanol was 97.1% by liquid chromatography analysis.

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PUM

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Abstract

The invention discloses a method for preparing campestanol by catalytic hydrogenation of ergosterol, and belongs to the technical field of goods, medicines, chemical industry, cosmetics and the like. The method comprises the following steps of dissolving ergosterol serving as a raw material into an organic solvent; performing catalytic hydrogenation with a hydrogenation catalyst under a certain temperature and pressure and at a certain agitating speed; and simply separating to obtain high-purity campestanol. The method is characterized in that ergosterol is used as the raw material and is processed by chemical hydrogenation to prepare mass campestanol; the ergosterol can be industrially produced, thus mass production of campestanol is realized. The method is simple in process, relatively low in cost, and efficient, simple and green in synthesis path.

Description

technical field [0001] The invention relates to a method for preparing campestanol by catalytic hydrogenation of ergosterol, which belongs to the technical fields of food, medicine, chemical industry and cosmetics. Background of the invention [0002] Phytosterol is an important active ingredient in plants, which has many important physiological functions such as lowering cholesterol, anti-tumor, and anti-inflammation. Phytosterols mainly include β-sitosterol, stigmasterol, campesterol, and brassicasterol. Phytostanols are phytosterols that do not contain carbon-carbon unsaturated bonds, mainly including sitostanol and campestanol. Compared with phytosterols, phytostanols have similar or even better physiological functions. [0003] Separation of phytosterol through multiple recrystallization methods can obtain pure β-sitosterol or stigmasterol, and hydrogenation of pure β-sitosterol or / and stigmasterol can produce sitosterol. CN1594351A discloses a method for preparing ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
Inventor 何文森孙俊张海晖胡迪
Owner JIANGSU UNIV
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