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Preparation method of m-nitroacetophenone

A kind of technology of nitroacetophenone and manufacturing method, applied in directions such as nitro compound preparation, organic chemistry and the like

Inactive Publication Date: 2011-06-01
高存元
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The advantage is that this technology suppresses the generation of o-p nitroacetophenone to the greatest extent, makes the product purified, solves the problem of carbonization in the nitration process, reduces the amount of by-products generated, and solves the comprehensive utilization of separated waste acid question

Method used

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  • Preparation method of m-nitroacetophenone
  • Preparation method of m-nitroacetophenone

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Embodiment Construction

[0006] The technical features of the present invention will be further described below in conjunction with the accompanying drawings and specific embodiments.

[0007] Referring to the attached figure, the 98% H 2 SO 4 Add catalyst and catalyst into the reaction kettle, start stirring, cool down to -8℃~-20℃, add acetophenone to keep the temperature, and slowly add the nitrating agent composed of concentrated nitric acid and concentrated sulfuric acid. During the dropping process, the temperature should be controlled at - Below 8°C, keep stirring for 20-40min, then slowly transfer the reactant to a reaction kettle containing a large amount of ice water under stirring, and control the temperature within 20°C-30°C during the transfer process; the product is solid , washed with clean water to remove acidic substances, then recrystallized with methanol, and finally obtained m-nitroacetophenone product with a purity of ≥99% through alcohol analysis. The dilute acid after centrifug...

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Abstract

The invention discloses a preparation method of m-nitroacetophenone, which comprises the steps of: with acetophenone as a raw material, reacting the acetophenone with concentrated sulfuric acid as a solvent to generate the m-nitroacetophenone by using copper salts with high selectivity as a catalyst under the action of the catalyst and the concentrated sulfuric acid as the solvent; and rapidly transferring reaction liquid into ice water, separating by using a centrifugal machine to obtain a crude product, recrystallizing the crude product with methyl alcohol, drying to obtain the m-nitroacetophenone, and centrifugally separating reacted acid and recycling. The m-nitroacetophenone is synthesized by adopting direct nitrification, thus the generation of the o-para nitroacetophenone can be furthest inhibited so that the product is purified, the carbonization problem in a nitrifying process is solved, the generation amount of side products is reduced and the problem of comprehensive utilization of separated reacted acid is solved at the same time.

Description

technical field [0001] The present invention relates to a kind of manufacture method of producing m-nitroacetophenone. Background technique [0002] m-Nitroacetophenone is one of the widely used intermediates in the chemical and pharmaceutical industries. At present, domestic and foreign synthetic industrial routes include the extraction method of chloramphenicol production waste liquid and the oxidation method of m-nitrophenylethylbenzene. Chloramphenicol production waste liquid extraction method uses waste liquid as raw material to obtain m-nitroacetophenone through concentration, decolorization, and multiple recrystallization. The problem of this process is insufficient raw material source, low product quality, high cost, and large environmental pollution; Using m-nitrobenzyl chloride as the starting material, generate m-nitroethylbenzene through lattice reaction, then generate m-nitroacetophenone through catalytic oxidation, and then purify the product through recrystal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/45C07C201/08
Inventor 高存元
Owner 高存元