A kind of preparation method of 5-aminosalicylic acid

A technology of aminosalicylic acid and nitrosalicylic acid, which is applied in the preparation of nitro compounds, organic compounds, cyanide reaction, etc., can solve the problem of severe exothermic heat of nitration reaction, a large amount of waste acid and iron powder, and safety Production hidden dangers and other problems, to achieve the effect of controllable heat release, improved utilization rate, and improved safety

Inactive Publication Date: 2018-05-15
HEILONGJIANG HAOYUN FINE CHEM
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] But there are following defects in the synthetic method of 5-aminosalicylic acid at present: 1, the exothermic heat of nitration reaction is violent, there is certain hidden danger of safe production in industrial large-scale production; 2, can produce a large amount of structural isomers in the reaction process, The ratio of the target product and the structural isomer is close to 1:1, and the chemical properties of the two are very similar so that the purification is difficult, the yield is reduced, and the total yield of the reaction is lower than 30%; 3, 5-aminosalicylic acid in the prior art The synthesis of iron powder will also use concentrated hydrochloric acid, resulting in a large amount of waste acid and iron powder, causing environmental pollution, etc.

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
  • A kind of preparation method of 5-aminosalicylic acid
  • A kind of preparation method of 5-aminosalicylic acid
  • A kind of preparation method of 5-aminosalicylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Weigh 80g of salicylic acid dissolved in 800ml of acetic acid as material 1, the molar concentration of salicylic acid in material 1 is 0.72mol / L; weigh 120g of concentrated nitric acid dissolved in 300ml of acetic acid as material 2, The molar concentration of nitric acid in material 2 is 3.2mol / L; 100ml of concentrated sulfuric acid is measured as material 3. The concentrated sulfuric acid is conventional commercial concentrated sulfuric acid, and the molar concentration is 18mol / L;

[0043] The flow rate of control material 1 is 22ml / min; the flow rate of control material 2 is 12ml / min; the flow rate of control material 3 is 6ml / min, and the material 1 is preheated to the reaction temperature in the first preheating module 11, and the material 2 and material 3 are in the second The preheating module 12 is mixed and preheated to the reaction temperature; then the material 1, the material 2 and the material 3 flow into the first reaction module 13, and the first reacti...

Embodiment 2

[0048] (1) Weigh 100 g of salicylic acid dissolved in 1000 ml of acetic acid as material 1, and the molar concentration of salicylic acid in material 1 is 0.72 mol / L; weigh 150 g of concentrated nitric acid and dissolve in 375 ml of acetic acid as material 2, The molar concentration of nitric acid in material 2 is 3.2 mol / L; 120ml of concentrated sulfuric acid is measured as material 3. The concentrated sulfuric acid is conventional commercial concentrated sulfuric acid, and the molar concentration is 18 mol / L;

[0049] Control the flow rate of material 1 to 20ml / min; control the flow rate of material 2 to 10ml / min; control the flow rate of material 3 to 5ml / min, the material 1 is preheated to the reaction temperature in the first preheating module 11, and the material 2 and material 3 are in the second The preheating module 12 is mixed and preheated to the reaction temperature; then the material 1, the material 2 and the material 3 flow into the first reaction module 13, where th...

Embodiment 3

[0054] (1) Weigh 90g of salicylic acid dissolved in 900ml of acetic acid as material 1. The molar concentration of salicylic acid in material 1 is 0.72mol / L; weigh 150g of concentrated nitric acid and dissolve in 375ml of acetic acid as material 2. The molar concentration of nitric acid in material 2 is 3.2 mol / L; 120ml of concentrated sulfuric acid is measured as material 3. The concentrated sulfuric acid is conventional commercial concentrated sulfuric acid, and the molar concentration is 18 mol / L;

[0055] Control the flow rate of material 1 to 25ml / min; control the flow rate of material 2 to 12ml / min; control the flow rate of material 3 to 6ml / min, material 1 is preheated to the reaction temperature in the first pre-heat preservation module 11, and material 2 and material 3 are in the second The preheating module 12 is mixed and preheated to the reaction temperature; then the material 1, the material 2 and the material 3 flow into the first reaction module 13, where they are u...

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 preparation method of 5-aminosalicylic acid. The method comprises the following steps: 1, preparing 5-nitrosalicylic acid: pre-incubating a salicylic acid solution used as a material 1, a concentrated nitric acid solution used as a material 2 and concentrated sulfuric acid used as a material 3 to a reaction temperature, mixing and reacting the material 1, the material 2 and the material 3, and post-processing the obtained reaction product to obtain purified 5-nitrosalicylic acid; and 2, preparing 5-aminosalicylic acid: dissolving the purified 5-nitrosalicylic acid in a solvent, adding Na2CO3 and a catalyst PdC to obtain a material 4, and carrying out pre-incubation catalytic hydrogenation to reduce the 5-nitrosalicylic acid into 5-aminosalicylic acid. The method has the advantages of simplicity in operation, controllable heat release, short production period, good area selectivity, environmental protection and safety, and realization of high yield and high purity of the finally obtained product.

Description

Technical field [0001] The invention relates to an organic synthesis method, in particular to a preparation method of 5-aminosalicylic acid. Background technique [0002] 5-Aminosalicylic acid (5-ASA, the drug name is mesalazine, also known as masalazine) is the main raw material and active ingredient of sulfasalazine for the treatment of chronic colitis and ulcerative colitis. By inhibiting the synthesis of prostaglandins that cause inflammation and the formation of inflammatory mediator leukotrienes, it significantly inhibits the inflammation of the intestinal mucosa and reduces the release of PGE2 in the human colonic mucosa. [0003] On the other hand, because 5-aminosalicylic acid has three active and reactive groups on the ring: amino, hydroxyl and carboxyl, it can undergo a variety of reactions. Therefore, in the dye industry, it can be used to produce a variety of excellent quality Reactive dyes. [0004] However, the current synthesis method of 5-aminosalicylic acid has th...

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 Patents(China)
IPC IPC(8): C07C227/04C07C229/64
CPCC07C201/08C07C227/04C07C229/64C07C205/59
Inventor 杨昆安永生
Owner HEILONGJIANG HAOYUN FINE CHEM
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap