Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Novel method for preparing 3-hydroxylquinaldine-4-carboxylic acid

A new method, the technology of hydroxyquinaldine, applied in the high-purity field, can solve the problems of dye dispersibility, poor level dyeing, low dye strength, 3-hydroxyquinaldine-4 carboxylic acid content, low purity, etc.

Active Publication Date: 2011-05-25
JIANGSU D I A N CHEM CO LTD
View PDF2 Cites 10 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The method is simple to operate, high in yield, and suitable for industrialized production, but the content and purity of 3-hydroxyquinaldine-4 carboxylic acid are low
Contains a large amount of inorganic salts, resulting in the subsequent production of disperse yellow 54, 64 and other dyes with low strength, poor frosting effect, poor dispersibility and level dyeing of dyes

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
  • Novel method for preparing 3-hydroxylquinaldine-4-carboxylic acid
  • Novel method for preparing 3-hydroxylquinaldine-4-carboxylic acid
  • Novel method for preparing 3-hydroxylquinaldine-4-carboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: 1. Take 1.0 mol of solid isatin, add it to 1224 ml of clear water, stir to dissolve, and filter out insoluble solids, add 1.0 mol of sodium hydroxide, mix and dissolve, filter, and collect the filtrate;

[0021] 2. Add 1.0 mol of sodium hydroxide to the obtained filtrate, dropwise add 1.0 mol of monochloroacetone, and dropwise add hydrochloric acid to adjust PH=7, then discharge and filter, collect the filter cake, and dry to obtain 196.96 grams of dry matter , detected by high-pressure liquid chromatography (HPLC), the purity is 98%, the yield is 95%, and the dissolution temperature is controlled between 10-80°C.

Embodiment 2

[0022] Embodiment 2: the consumption of monochloroacetone is increased to 1.5mol, and dissolution temperature is controlled between 45~55 ℃, repeats embodiment 1, obtains 196.37 grams of dry matter, detects through high pressure liquid chromatography (HPLC), and purity is 98.5%, the yield is 95.2%, and the dissolution temperature is controlled between 10-80°C.

Embodiment 3

[0023] Embodiment 3: the consumption of monochloroacetone is increased to 2mol, and dissolution temperature is controlled between 45~55 ℃, repeats Example 1, obtains 200.05 grams of dry matter, detects through high-pressure liquid chromatography (HPLC), and purity is 97.5 %, the yield is 96%.

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 relates to a novel method for preparing 3-hydroxylquinaldine-4-carboxylic acid. The 3-hydroxylquinaldine-4-carboxylic acid produced by the prior art has low purity. To solve the problem, the novel method for preparing the 3-hydroxylquinaldine-4-carboxylic acid comprises the following steps of: (1) adding 1.0 molar part of solid isatin into enough clear water, then adding 1.0 equivalent molar part of inorganic base, mixing and dissolving, filtering, and collecting filtrate; and (2) adding 1.0 equivalent molar part of inorganic base into the obtained filtrate, dropwise adding 1 to2.0 molar parts of monochloroacetone, then dropwise adding hydrochloric acid to adjust the pH value to be 7, then emptying and filtering, collecting a filter cake, and drying to obtain a finished product. BY the method, the content and purity of the 3-hydroxylquinaldine-4-carboxylic acid are improved on the premise of not increasing equipment, raw materials, processes and the like; and the purityof the 3-hydroxylquinaldine-4-carboxylic acid prepared by the method is over 97 percent, and the yield is more than or equal to 95 percent.

Description

technical field [0001] The invention relates to a new method for preparing 3-hydroxyquinaldine-4-carboxylic acid, which is especially suitable for the preparation of high-purity and high-content quinaldine. Background technique [0002] 3-Hydroxyquinaldine-4-carboxylic acid is the main intermediate for the preparation of C.I. Disperse Yellow 54 and 64. It is also a pharmaceutical intermediate. In conventional production technology, the process of synthesizing 3-hydroxyquinaldine-4-carboxylic acid with isatin as raw material is very mature. The process mainly includes the following steps: [0003] 1. The reaction of monochloroacetone and calcium hydroxide generates 1-hydroxyacetone, and its characteristics are as follows: [0004] [0005] 2. Isatin is ring-opened and dissolved under alkaline conditions, and its characteristics are as follows: [0006] [0007] 3. The product of step 1 and the product of step 2 are reacted in an aqueous medium, and the characteristi...

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): C07D215/50
Inventor 陶国来
Owner JIANGSU D I A N CHEM CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com