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Method for preparing gossypol acetate based on solid phase synthesis

A technology of gossypol acetate and solid-phase synthesis, which is applied in the chemical field, can solve problems such as toxic residues and affecting applications, and achieve the effects of low cost, reduced usage, and high extraction rate

Inactive Publication Date: 2015-06-10
ANYANG NORMAL UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to improve the extraction rate of gossypol acetate, aniline and gossypol are often used to react to generate Schiff base, and then acid hydrolysis is used to obtain gossypol acetate. A small amount of aniline will remain in the gossypol acetate product by this preparation method, causing toxic residues. Thus affecting its application in the field of medicine and other fields with high purity requirements

Method used

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  • Method for preparing gossypol acetate based on solid phase synthesis
  • Method for preparing gossypol acetate based on solid phase synthesis
  • Method for preparing gossypol acetate based on solid phase synthesis

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Weigh 20 g of cottonseed powder, wrap it in a filter paper tube, place it in a Soxhlet extractor, and add 150 mL of acetone to reflux for extraction for 12 h. Add 20 g of treated D380 amino resin to the extract, and stir for 4 h at room temperature. After the reaction was completed, suction filtered, and the amino resin bonded with gossypol was washed several times with petroleum ether and distilled water, then the resin was transferred to a 250 mL flat-bottomed flask, and a mixture of 60 mL of acetone and glacial acetic acid at a volume ratio of 1:1 was added. Turn on the magnetic stirring, slowly add 5 mL of sulfuric acid with a mass fraction of 9% with a dropping funnel, and stir at room temperature for 24 h. Suction filtration under reduced pressure, and the filtrate was concentrated to 20 mL at 55°C under reduced pressure, and then placed in the refrigerator overnight, and gossypol acetate solids were precipitated, filtered by suction, washed with petroleum ether a...

Embodiment 2

[0030] Weigh 20 g of cottonseed powder, wrap it in a filter paper tube, place it in a Soxhlet extractor, and add 150 mL of acetone to reflux for extraction for 12 h. Add 20 g of treated D392 amino resin to the extract, and stir for 4 h at room temperature. After the reaction, the amino resin bound to gossypol was washed with petroleum ether and distilled water for several times, then transferred to a 250 mL flat-bottomed flask, and 60 mL of a mixture of acetone and glacial acetic acid (volume ratio 1:1 ), turn on the magnetic stirring, slowly add 5 mL of sulfuric acid with a mass fraction of 9% using a dropping funnel, and stir at room temperature for 24 h. Suction filtration under reduced pressure, the filtrate was concentrated under reduced pressure at 55 °C to 20 mL, and then placed in the refrigerator overnight, gossypol acetate solids were precipitated, filtered by suction, washed with petroleum ether and distilled water in sequence, and dried to obtain 155 mg gossypol ac...

Embodiment 3

[0032] Weigh 20 g of cottonseed powder, wrap it in a filter paper tube, place it in a Soxhlet extractor, and add 150 mL of ethyl acetate to reflux for extraction for 12 h. Add 20 g of treated D380 amino resin to the extract, and stir for 4 h at room temperature. After the reaction, the amino resin bound to gossypol was washed with petroleum ether and distilled water for several times, then transferred to a 250 mL flat-bottomed flask, and 60 mL of a mixture of acetone and glacial acetic acid (volume ratio 1:1 ), turn on the magnetic stirring, slowly add 5 mL of sulfuric acid with a mass fraction of 9% using a dropping funnel, and stir at room temperature for 24 h. Suction filtration under reduced pressure, the filtrate was concentrated to 20 mL under reduced pressure at 55 °C, and then placed in the refrigerator overnight, gossypol acetate solids were precipitated, filtered by suction, washed with petroleum ether and distilled water in sequence, and dried to obtain 117 mg gossy...

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Abstract

The invention discloses a method for preparing gossypol acetate based on solid phase synthesis, belonging to the field of chemistry. The method comprises the following steps: by taking cotton seed power as a raw material, performing solvent extraction, and resin bonding and adsorption, analyzing acetic acid, filtering, concentrating, and washing to obtain high-concentration gossypol acetate. The gossypol acetate is prepared by adopting a solid phase synthesis technology, the raw materials do not need to be degreased, and the purity of the gossypol acetate can achieve 100%. According to the method, the preparation technology of the gossypol acetate is shortened, the usage amount of the solvent is reduced on a large scale, the use of aniline can be avoided, and the residual toxicity problems of aniline on the surface of the gossypol acetate can be overcome.

Description

technical field [0001] The invention relates to a method for preparing gossypol acetate, in particular to a method for preparing gossypol acetate based on solid-phase synthesis, and belongs to the chemical field. Background technique [0002] Gossypol acetate is a complex salt of gossypol and acetic acid, which is more stable than gossypol, and its molecular formula is C 32 h 34 o 10 , is a compound with a wide range of pharmacological effects. As early as the 1970s, Chinese researchers discovered that gossypol had the effect of male birth control, which aroused widespread interest of scholars at home and abroad. In addition, gossypol acetate has certain curative effects in treating climacteric women's diseases, anti-tuberculosis, anti-tumor and anti-virus. Not only that, gossypol acetate has good application in many fields such as industry, pesticide, petroleum, chemical industry, etc., and its application prospect is very wide. Common process methods for preparing gos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/21C07C67/48C07C67/56
Inventor 吴汉夔王森胜胥盈盈杨伟华
Owner ANYANG NORMAL UNIV
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