Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for preparing 5-aminosalicylic acid

A technology of aminosalicylic acid and sodium aminosalicylate, applied in chemical instruments and methods, cyanide reaction preparation, preparation of organic compounds, etc., can solve the problems of harsh reaction conditions, low pollution, short process routes, etc. Mild reaction conditions, safe production and good reaction selectivity

Inactive Publication Date: 2012-10-17
HUNAN KAIMEITE GASES
View PDF2 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This document simply reports that the total yield of 5-ASA prepared by this method is over 80%. This method has a short process route and less pollution, but the reaction conditions are harsh, and the gas-solid carboxylation reaction is carried out under high temperature and pressure, and aminophenol is easily destroyed Oxidation and polymerization

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing 5-aminosalicylic acid
  • Method for preparing 5-aminosalicylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 2.0g of the substrate sodium p-aminophenate and put it into a 50ml autoclave, add 13.54g of ionic liquid 1-butyl-3-methylimidazole chloride, seal the autoclave with a lid, and feed CO2 gas for carboxylation Carboxylation reaction, when the reaction temperature is 140°C and the reaction pressure is 2.5MPa, maintain the pressure and temperature, continue the carboxylation reaction for 10 hours, and obtain a reaction mixture containing sodium 5-aminosalicylate; stop the carboxylation reaction, and pass through condensing Water makes the temperature in the autoclave drop below 80°C quickly, and at the same time, open the air valve to discharge the carbon dioxide gas in the high-pressure reaction kettle. After the carbon dioxide gas is released, open the lid of the high-pressure reaction kettle; Reaction mixture to obtain a solution of the reaction mixture containing 5-aminosalicylate sodium; acidify the solution of the reaction mixture containing 5-aminosalicylate sodi...

Embodiment 2

[0029]Weigh 2.0g of the substrate sodium p-aminophenate and put it into a 50ml autoclave, add 13.54g of ionic liquid 1-butyl-3-methylimidazole chloride, seal the autoclave with a lid, and feed CO2 gas for carboxylation Carboxylation reaction, when the reaction temperature is 120°C and the reaction pressure is 3.0MPa, maintain the pressure and temperature, continue the carboxylation reaction for 10 hours, and obtain a reaction mixture containing sodium 5-aminosalicylate; stop the carboxylation reaction, and pass through condensing Water makes the temperature in the autoclave drop below 80°C quickly, and at the same time, open the air valve to discharge the carbon dioxide gas in the high-pressure reaction kettle. After the carbon dioxide gas is released, open the lid of the high-pressure reaction kettle; Reaction mixture to obtain a solution of the reaction mixture containing 5-aminosalicylate sodium; acidify the solution of the reaction mixture containing 5-aminosalicylate sodiu...

Embodiment 3

[0031] Weigh 2.0g of the substrate sodium p-aminophenate and put it into a 50ml autoclave, add 13.54g of ionic liquid 1-butyl-3-methylimidazole chloride, seal the autoclave with a lid, and feed CO2 gas for carboxylation Carboxylation reaction, when the reaction temperature is 200°C and the reaction pressure is 0.5MPa, maintain the pressure and temperature, continue the carboxylation reaction for 10 hours, and obtain a reaction mixture containing sodium 5-aminosalicylate; stop the carboxylation reaction, and pass through condensing Water makes the temperature in the autoclave drop below 80°C quickly, and at the same time, open the air valve to discharge the carbon dioxide gas in the high-pressure reaction kettle. After the carbon dioxide gas is released, open the lid of the high-pressure reaction kettle; Reaction mixture to obtain a solution of the reaction mixture containing 5-aminosalicylate sodium; acidify the solution of the reaction mixture containing 5-aminosalicylate sodi...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method for preparing 5-aminosalicylic acid. The method comprises the following steps of: adding an ionic liquid 1-butyl-3-methylimidazolium chloride and a substrate sodium p-aminophenolate into a reaction kettle; dissolving the sodium p-aminophenolate into the 1-butyl-3-methylimidazolium chloride to form solution; inputting carbon dioxide gas into the solution and making the carbon dioxide gas and the sodium p-aminophenolate fully generate the gas phase carboxylation, wherein the reaction pressure of the gas phase carboxylation is between 0.5MPa and 3MPa and the reaction temperature of the gas phase carboxylation is between 120 DEG C and 200 DEG C; obtaining a reaction mixture with sodium 5-aminosalicylate; dissolving the reaction mixture with sodium 5-aminosalicylate in water to obtain the solution of the reaction mixture with sodium 5-aminosalicylate; and, acidifying the solution of the reaction mixture with sodium 5-aminosalicylate by dilute hydrochloric acid to form acidified solution, and reacting the hydrochloric acid and sodium 5-aminosalicylate to generate the 5-aminosalicylic acid and separate the 5-aminosalicylic acid from the acidified solution.

Description

【Technical field】 [0001] The present invention generally relates to the preparation method of phenolic acid, especially a kind of method of preparation 5-amino salicylic acid. 【Background technique】 [0002] 5-Amino salicylic acid (5-Amino salicylic acid), the trade name is melasalazine, because 5-amino salicylic acid (5-ASA) has free radical (DPPHL) reduction, hydrogen peroxide elimination, secondary Chlorate ion elimination, lipid peroxide inhibition and leukotriene B4 biosynthesis inhibition, mainly used in pharmaceutical, pesticide and other industrial fields. [0003] Ulcerative colitis is a non-specific chronic intestinal disease, which cannot be completely cured so far. Currently, 5-aminosalicylic acid and its derivatives are the drugs of choice for the treatment of this disease. Currently, there are four main synthetic methods of 5-ASA reported in the literature: aniline method, salicylic acid method, p-aminophenol solid-phase carboxylation synthesis method and ace...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/64C07C227/16
Inventor 刘志刚吉琳韬祝恩福李媛媛汪秋安张晓辉尹双凤张伟李文盛
Owner HUNAN KAIMEITE GASES