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A method for preparing free gossypol with gossypol acetate as raw material

A technology of gossypol acetate and free gossypol, applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve the problems of industrial equipment corrosion, unfavorable drug preparation, and increased cost, and achieve easy preservation and The effect of short transportation and preparation time and increased cost

Inactive Publication Date: 2021-03-09
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires the use of corrosive sulfuric acid, and the raw materials used contain highly toxic diphenylamine, which is not conducive to drug production
And the method that has been reported to prepare gossypol from gossypol acetate all cannot do without the use of alkali, and these alkaline substances such as lye, sodium carbonate, sodium bisulfite, borate, hydrosulfite (sodium dithionite) etc. have Certain toxic and side effects have certain corrosiveness to industrial equipment, and correspondingly increase the cost. Therefore, the preparation of free gossypol needs to start from the selection of raw materials, and choose low-cost, stable properties, and low toxic and side effects raw materials as much as possible, and then use The production process is as simple and efficient as possible to reduce the production cost of gossypol, and prepare high-purity free gossypol on the basis of ensuring that gossypol is an aldehyde structure, so as to improve medical value and broaden the application field

Method used

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  • A method for preparing free gossypol with gossypol acetate as raw material
  • A method for preparing free gossypol with gossypol acetate as raw material
  • A method for preparing free gossypol with gossypol acetate as raw material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] a, the dissolving of crude gossypol acetate: take by weighing 1g of crude gossypol acetate with a purity of 80% and dissolve it in 20ml organic solvent as freshly distilled ether to obtain the mixed solution;

[0043] b. Ultrasonic extraction of crude gossypol: add 10ml of distilled water to the mixed solution obtained in step a for ultrasonication, the ultrasonic frequency is 22kHz, the ultrasonic power is 300W, the ultrasonic time is 10s, the interval time is 10s, the ultrasonic temperature is 25°C, and the duration is 10min After standing still, the mixed solution is layered, the distilled water is removed, and this step is repeated twice to obtain the mixed solution;

[0044] c. Recrystallization of free gossypol: at room temperature, concentrate the mixed solution obtained in step b under reduced pressure to 1 / 2 of the volume of the initial mixed solution in step b, then slowly add petroleum ether with a low boiling point of 30-60°C , and shake gently until the mix...

Embodiment 2

[0046] a, the dissolving of crude gossypol acetate: take by weighing 1g of crude gossypol acetate with a purity of 80% and dissolve it in 20ml organic solvent as freshly distilled ether to obtain the mixed solution;

[0047] b. Ultrasonic extraction of crude gossypol: add 6ml of distilled water to the mixed solution obtained in step a for ultrasonication, the ultrasonic frequency is 22kHz, the ultrasonic power is 300W, the ultrasonic time is 10s, the interval time is 10s, the ultrasonic temperature is 30°C, and the duration is 10min After standing still, the mixed solution is layered, the distilled water is removed, and this step is repeated twice to obtain the mixed solution;

[0048] c. Recrystallization of free gossypol: at room temperature, concentrate the mixed solution obtained in step b under reduced pressure to 1 / 2 of the volume of the initial mixed solution in step b, then slowly add petroleum ether with a low boiling point of 30-60°C , and shake gently until the mixe...

Embodiment 3

[0050] a, the dissolving of crude gossypol acetate: take by weighing 1g of crude gossypol acetate with a purity of 80% and dissolve it in 20ml organic solvent as freshly distilled ether to obtain the mixed solution;

[0051] b. Ultrasonic extraction of crude gossypol: add 10ml of saturated saline to the mixed solution obtained in step a for ultrasonication, ultrasonic frequency 22kHz, ultrasonic power 300W, ultrasonic time 10s, interval time 10s, ultrasonic temperature 30°C, continue After standing still for 10 minutes, the mixed solution was layered, and the saturated saline solution was removed, and this step was repeated twice to obtain the mixed solution;

[0052] c. Recrystallization of free gossypol: at room temperature, concentrate the mixed solution obtained in step b under reduced pressure to 1 / 2 of the volume of the initial mixed solution in step b, then slowly add petroleum ether with a low boiling point of 30-60°C , and shake gently until the mixed solution starts ...

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Abstract

The invention relates to a method for preparing free gossypol by using gossypol acetate as a raw material. The method destroys the intermolecular hydrogen bond between acetic acid and gossypol in gossypol acetate by ultrasonic waves, and then allows the acetic acid to enter the aqueous solution or saturated saline solution, Realize the separation of free gossypol and acetic acid, recrystallize the crude free gossypol to obtain high-purity free gossypol, the whole preparation process is carried out at room temperature, and the preparation time is short, effectively avoiding gossypol structural oxidation and various isomerization The method has the advantages of low cost of raw materials, short process flow, good repeatability, high purity, high safety, short time and high efficiency. The invention has certain economic value and practical value.

Description

technical field [0001] The invention relates to a method for preparing free gossypol by using gossypol acetate as a raw material, belonging to the field of fine chemicals. Background technique [0002] Gossypol, also known as gossypol, is a yellow polyphenolic hydroxyl bisnaphthaldehyde compound, which widely exists in the roots, stems, leaves and seeds of Malvaceae plants, especially in cottonseed kernels. Since the 1970s, Chinese researchers first discovered that gossypol has the effect of inhibiting spermatogenesis and sperm motility, and it can be used as a male contraceptive in clinical practice. Researchers from various countries have conducted extensive research on the application of gossypol and its derivatives , found that gossypol and its derivatives have broad application prospects in medicine, health, agriculture, chemical industry, genetic engineering, etc. For example, in the chemical industry, gossypol can be used as antioxidants, stabilizers, polymerization i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/61C07C45/81C07C47/57
CPCC07C45/61C07C45/81C07C47/57
Inventor 张亚刚陈玉荣王璐璐张乐涛艾克热木·牙生姜莹芳郅柯柯
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI