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Production method of 8-hydroxyquinoline

A technology of hydroxyquinoline and production method, applied in the direction of organic chemistry, etc., can solve the problems of 8-hydroxyquinoline product yield and quality impact, poor product quality, low product yield, etc.

Inactive Publication Date: 2020-10-20
菏泽鸿特药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] Because the side reaction of above-mentioned existence can influence the yield and the quality of 8-hydroxyquinoline product, therefore, the production technology of traditional 8-hydroxyquinoline has problems such as low product yield and poor product quality

Method used

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  • Production method of 8-hydroxyquinoline
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  • Production method of 8-hydroxyquinoline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] as attached figure 1 Shown, this embodiment provides a kind of production method of 8-hydroxyquinoline, it may further comprise the steps:

[0034] S1. After putting 168kg of o-aminophenol and 102kg of o-nitrophenol into the mixing kettle, add 340kg of 98% sulfuric acid dropwise into the mixing kettle. After the dropwise addition, stir and mix for half an hour. During the stirring process, the temperature should be controlled at 70 °C, after the stirring and mixing are completed, a mixture is obtained.

[0035] S2. Vacuum transfer the above mixture to the synthesis kettle, then, drop 230kg of glycerin in the metering tank into the synthesis kettle (dropping is completed within 8 hours), and heat up to 150°C through the jacket of the synthesis kettle to carry out The cyclization reaction was carried out for 4 hours. After the reaction was completed, circulating cooling water was passed through the jacket of the synthesis kettle to lower the temperature of the material t...

Embodiment 2

[0039] This embodiment provides a kind of production method of 8-hydroxyquinoline, it may further comprise the steps:

[0040] S1. After putting 168kg of o-aminophenol and 84kg of o-nitrophenol into the mixing kettle, add 302.4kg of 98% sulfuric acid dropwise into the mixing kettle. After the addition, stir and mix for half an hour. 60°C, after stirring and mixing, a mixture was obtained.

[0041] S2. Vacuum transfer the above mixture to the synthesis kettle, then add 201.6kg of glycerin in the metering tank dropwise into the synthesis kettle (the addition is completed within 8 hours), and heat up to 140°C through the jacket of the synthesis kettle The cyclization reaction was carried out for 4 hours. After the reaction was completed, circulating cooling water was passed through the jacket of the synthesis kettle to lower the temperature of the material to 80° C. to obtain a reaction solution.

[0042] S3. Pump the above reaction solution into the neutralization kettle, then ...

Embodiment 3

[0045] This embodiment provides a kind of production method of 8-hydroxyquinoline, it may further comprise the steps:

[0046] S1. After putting 168kg of o-aminophenol and 117.6kg of o-nitrophenol into the mixing kettle, add 369.6kg of 95% sulfuric acid dropwise into the mixing kettle. After the dropwise addition, stir and mix for half an hour. The temperature needs to be controlled during the stirring process After stirring and mixing at 80° C., a mixture was obtained.

[0047] S2. Vacuum transfer the above mixture to the synthesis kettle, then add 252kg of glycerin in the metering tank dropwise into the synthesis kettle (the dropwise addition is completed within 8 hours), and heat up to 160°C through the jacket of the synthesis kettle to carry out The cyclization reaction was carried out for 4 hours. After the reaction was completed, circulating cooling water was passed through the jacket of the synthesis kettle to lower the temperature of the material to 80° C. to obtain a ...

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Abstract

The invention is applicable to the technical field of chemical industry production, and provides a production method of 8-hydroxyquinoline. The method comprises the following steps: stirring and mixing o-aminophenol, o-nitrophenol and an acid solution to obtain a mixture; dropwise adding glycerol into the mixture, and carrying out a cyclization reaction to obtain a reaction solution; neutralizingthe reaction solution with an alkali liquid until the pH value is 7-8, and separating to obtain an organic phase; and carrying out water washing and layering on the organic phase, and then sequentially carrying out reduced pressure distillation, condensation and crushing treatment to obtain the 8-hydroxyquinoline. According to the method, o-aminophenol and o-nitrophenol are firstly added, concentrated sulfuric acid is dropwise added, and then glycerol is added, so that the product can be directly synthesized by a one-pot method, the production method effectively reduces side reactions, the yield and the quality of the 8-hydroxyquinoline product are further improved, the product conversion rate can reach 96%, and the product yield can reach 91%.

Description

technical field [0001] The invention belongs to the technical field of chemical production, in particular to a production method of 8-hydroxyquinoline. Background technique [0002] 8-Hydroxyquinoline, which can be used as a pharmaceutical intermediate, is the raw material for the synthesis of Kexielunin, clioquinoline, and phantomine, and is also an intermediate for dyes and pesticides. [0003] In the prior art, 8-hydroxyquinoline can be synthesized by using o-aminophenol, o-nitrophenol and glycerol as main raw materials, and its synthetic route and reaction principle are as follows: [0004] (1) Synthesis of acrolein reaction: [0005] ; [0006] (2) Synthesis of 8-hydroxy-1,2-dihydroquinoline: [0007] ; [0008] (3) Synthesis of 8-hydroxy-1,2-dihydroquinoline: [0009] ; [0010] (4) Acid-base neutralization. [0011] Among them, the production process of traditional 8-hydroxyquinoline is generally to add glycerin and drop concentrated sulfuric acid first. ...

Claims

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Application Information

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IPC IPC(8): C07D215/26
CPCC07D215/26
Inventor 殷文
Owner 菏泽鸿特药业有限公司
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