Preparation method of diacerein

A technology of diacerein and sodium acetate, which is applied in the field of preparation of diacerein, can solve the problems of insufficient sources, inapplicability to industrialized large-scale production, and many pollutants, so as to reduce the discharge of three wastes, improve production efficiency, Effect of Simplified Preparation Method

Active Publication Date: 2021-01-29
SHAANXI JIAHE PHYTOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention solves the problem that the current total synthesis method for preparing diacerein has many steps, the raw materials are expensive and the source is insufficient, and the reagents and auxiliary materials used are highly toxic and are not suitable for Industrialized large-scale production, but the key oxidation system in the semi-synthetic method has potential safety hazards, the amount of oxidant and reaction solvent used is large and produces many pollutants, and the technical problems of low profit margin of the product. A preparation method for diacerein is provided

Method used

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  • Preparation method of diacerein
  • Preparation method of diacerein
  • Preparation method of diacerein

Examples

Experimental program
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Effect test

Embodiment 1

[0051] Add 250kg of glacial acetic acid and 100kg of triacetyl aloe-emodin in the reaction tank, start stirring, and open cold brine to cool down. In the batching tank, add 22kg of manganese chloride tetrahydrate, 22kg of water, stir and dissolve; continue to put in 35kg of chromic anhydride, 23kg of sodium acetate, and 210kg of 85% glacial acetic acid, stir for 40 minutes at normal temperature, and the solid is dissolved and clear, and pumped into the high-level tank for standby. At this time, the temperature in the reaction tank dropped to 0°C, and the cold brine inlet and outlet valves were closed. Close the high-level tank emptying valve, open the compressed air valve, when the pressure in the tank is 0.1mpa, open the high-level tank bottom valve, and quickly press the oxidant into the oxidation tank. When the pressure is 0, close the high-level tank bottom valve, and when the pressure returns to 0.1mpa Then open it quickly, close the compressed air valve when the pressure...

Embodiment 2

[0054] Add 300kg of glacial acetic acid and 100kg of triacetyl aloe-emodin in the reaction tank, start stirring, and open cold brine to cool down. In the batching tank, add 25kg of manganese chloride tetrahydrate and 25kg of water, stir and dissolve. Continue to put in 40kg of chromic anhydride, 25kg of sodium acetate, 250kg of 85% glacial acetic acid, stir at normal temperature for 30 minutes, the solid is dissolved and clear, and pumped into the overhead tank for subsequent use. At this time, the temperature in the reaction tank dropped to 0°C, and the cold brine inlet and outlet valves were closed. Close the high-level tank emptying valve, open the compressed air valve, when the pressure in the tank is 0.1mpa, open the high-level tank bottom valve, and quickly press the oxidant into the oxidation tank. When the pressure is 0, close the high-level tank bottom valve, and when the pressure returns to 0.1mpa Then open it quickly, close the compressed air valve when the pressur...

Embodiment 3

[0057] Add 350kg of glacial acetic acid and 100kg of triacetyl aloe-emodin in the reaction tank, start stirring, and open cold brine to cool down. In the batching tank, add 30kg manganese chloride tetrahydrate and 30kg water, stir and dissolve. Continue to drop into chromic anhydride 35kg, sodium acetate 25kg, concentration is 65% recovery glacial acetic acid 250kg, stir at normal temperature for 30 minutes, the solid is dissolved and clear, is pumped into the overhead tank for subsequent use. At this time, the temperature in the reaction tank dropped to 0°C, and the cold brine inlet and outlet valves were closed. Close the high-level tank emptying valve, open the compressed air valve, when the pressure in the tank is 0.1mpa, open the high-level tank bottom valve, and quickly press the oxidant into the oxidation tank. When the pressure is 0, close the high-level tank bottom valve, and when the pressure returns to 0.1mpa Then open it quickly, close the compressed air valve whe...

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Abstract

The invention relates to a semi-synthesis method of diacerein, and provides a preparation method of diacerein in order to solve the technical problems that an existing full-synthesis method for preparing diacerein has many steps, raw materials are expensive and insufficient in source, reagents and auxiliary materials are high in toxicity, and a key oxidation system in the semi-synthesis method ishigh in three-waste content. The preparation method comprises steps: mixing triacetyl aloe-emodin with glacial acetic acid to obtain a reaction raw material; adding a water-soluble manganese salt andwater, and stirring; adding chromic anhydride, sodium acetate and a glacial acetic acid solution, and stirring until a solution is dissolved and clarified to obtain an oxidizing agent; pressing the oxidizing agent into the reaction raw materials, controlling the temperature to be 95-110 DEG C for reaction; recovering glacial acetic acid under normal pressure and then reduced pressure, adding water, stirring and pulping, and centrifugalizing, washing with water to obtain a diacerein crude product; dissolving the diacerein crude product in an ethanol solution of sodium hydroxide, filtering, taking a liquid part, adjusting the pH value to 3-4, centrifuging after filtering, washing a solid part with water until the solid part is neutral, and drying to obtain diacerein.

Description

technical field [0001] The invention relates to a semi-synthetic method of diacerein, in particular to a preparation method of diacerein. Background technique [0002] Diacerein is an anthraquinone compound whose chemical name is 4,5-bis(acetoxy)-9,10-anthraquinone-2-carboxylic acid. Diacerein is a new interleukin (IL-1) inhibitor with the trade name of Ambidine. It is commonly used clinically to improve pain and bone and joint disorders caused by osteoarthritis and other related diseases, and can significantly improve bone and joint patients. It can improve the joint function, delay the course of disease and relieve pain. Its compound is a yellow needle-like solid, and its structural formula is as follows: [0003] [0004] There are many reports about the preparation method of diacerein, mainly two ways of total synthesis method and semi-synthesis method: (1) total synthesis method, Steve Tisserand etc. take m-tribromobenzene and o-methoxybenzoic acid as main raw mater...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/16C07C67/29C07C67/48C07C67/60
CPCC07C67/29C07C67/48C07C67/60C07C2603/24C07C69/16Y02P20/55
Inventor 肖金霞王金龙刘娜郭文华
Owner SHAANXI JIAHE PHYTOCHEM
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