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Preparation method of quinolone, isoquinoline and methylquinolines

A technology of methylquinoline and dimethylquinoline, applied in the direction of organic chemistry, can solve the problems of long methylquinoline extraction process and waste acid water, and achieve less additional raw materials, short process and low cost Effect

Active Publication Date: 2014-12-24
山西永东化工股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A method for extracting high-purity 4-methylquinoline (application number 201110190801.5), using solvent distillation and sulfuric acid reaction crystallization method to extract 6-methylquinoline (application number 201310044393.1) and 8-methylquinoline (application number 201310044468.6 ), but many methylquinoline extraction processes are long and prone to waste acid water

Method used

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Examples

Experimental program
Comparison scheme
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Embodiment Construction

[0014] (1) After rectification enrichment, quinoline 0.32-0.57Wt%, isoquinoline 70.33-78.80Wt%, 2, 3, 4, 6-methylquinoline 11.22-21.85Wt%, 2, 4-di The 5.18-7.55Wt% solution of methylquinoline is placed in the urea aqueous solution with a mass concentration of 2-15% at a temperature of 15-26°C to form a 99%, the remaining liquid quinoline returns to the quinoline raw material system;

[0015] (3) 21.80wt% of 2, 3, 4, 6-methylquinoline and other monomethylquinolines and 5.20wt% of 2,4-bis The methyl quinoline solution is frozen at a temperature of 5-10°C for 2-5 hours, and a variety of monomethyl quinoline and 2,4-dimethyl quinoline and mixed solvents outside the urea coronal clathrate are separated, and through the crystallization point The difference is to separate a variety of monomethylquinoline and 2,4-dimethylquinoline in the solid phase from the mixed solvent in the liquid state;

[0016] (4) Put the separated monomethylquinoline and 2,4-dimethylquinoline solid phases in...

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Abstract

The invention discloses a preparation method of quinolone, isoquinoline and methylquinolines, aiming to be short in process flow and low in cost. The preparation method comprises the following steps: placing rectified residual liquor obtained from extraction of quinolone into a urea coronary inclusion complex, and carrying quinolone and isoquinoline in a solution into the urea coronary inclusion complex according to molecule sizes; according to difference of crystallization points, separating the quinolone from isoquinoline; separating multiple solid-phase monomethylquinolone from a liquid-state mixed solvent; placing the separated multiple solid-phase monomethylquinoline and solid-phase 2,4-dimethylquinoline into a thiourea water solution for dipping to form a thiourea coronary inclusion complex; spraying anhydrous methanol, propanol, butanone and pentanone mixed solvent through a peristaltic pump; crystalizing 2,4-dimethylquinolone dissolved in the mixed solvent, separating from other trace polymethylquinolone impurities, and refining to obtain 2,4-dimethylquinoline products; and according to the difference of crystallization points, placing the thiourea coronary inclusion complex into a crystallization kettle for heating and separation.

Description

technical field [0001] The invention belongs to the field of petrochemical industry, and in particular relates to a method for preparing quinoline, isoquinoline and various methylquinolines. Background technique [0002] Coal tar is the main source of quinoline, isoquinoline and various methylquinolines in my country. In recent years, new drugs of quinoline, isoquinoline and various methylquinolines have been continuously developed in the pharmaceutical industry. From the original antimalarial drugs to local anesthetic drugs, from antibacterial and antifungal drugs to antitumor and anti-infectious disease drugs; in agriculture, from herbicides to fungicides and insecticides, they are not only effective but also have low toxicity and residue. In addition, quinoline, isoquinoline and methylquinoline are rubber anti-aging agents, photographic sensitizers, metal anti-corrosion agents, etc., and are widely used. However, the methods and techniques for extracting quinoline and m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/04C07D215/02C07D217/02
CPCC07D215/02C07D215/04C07D217/02
Inventor 刘东良刘东玉周霞萍
Owner 山西永东化工股份有限公司
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