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Preparation method of benzaldehyde

A technology of benzaldehyde and nitrobenzaldehyde, applied in the preparation of nitro compounds, organic chemistry, etc., can solve the problems of large environmental damage, poor o-para selectivity, and large amount of three wastes

Inactive Publication Date: 2019-12-10
枣阳市众成化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are very few domestic manufacturers. The reason is that the existing production process is complicated, the selectivity of the ortho-para position is poor, and qualified products need to be recrystallized many times. The high-purity products are not high and the amount of three wastes is large, which is very destructive to the environment. Big

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] S1: Add copper nitrate, water, silver nitrate and catalyst concentrated nitric acid into the reaction device, raise the temperature to 70°C, add benzaldehyde dropwise, the dropwise addition time is 2 hours, continue to heat up to 95°C, keep the temperature for 2 hours, Obtain reaction mixture, wherein the mol ratio of copper nitrate, water, silver nitrate, catalyst concentrated nitric acid and benzaldehyde is 5:40:1:0.2:1; Sampling is carried out chromatographic detection from reaction mixture, and the content of benzaldehyde is less than 0.5 %;

[0020] S2: Filter the reaction mixture to remove the copper hydroxide precipitate to obtain the mother liquor, cool the mother liquor to 20°C, and filter the solid to obtain the crude m-nitrobenzaldehyde, the content of o-nitrobenzaldehyde in the crude m-nitrobenzaldehyde less than 0.5%;

[0021] S3: Put the m-nitrobenzaldehyde crude product into the reaction device, add a water-soluble solvent methanol that is 3.0 times the ...

Embodiment 2

[0023] S1: Add copper nitrate, water, silver nitrate and catalyst concentrated nitric acid into the reaction device, raise the temperature to 80°C, add benzaldehyde dropwise, the dropwise addition time is 3 hours, continue to heat up to 85°C, and keep warm for 2.5 hours to react. Obtain reaction mixture, wherein the mol ratio of copper nitrate, water, silver nitrate, catalyst concentrated nitric acid and benzaldehyde is 5:40:1:0.2:1; Sampling is carried out chromatographic detection from reaction mixture, and the content of benzaldehyde is less than 0.5 %;

[0024] S2: Filter the reaction mixture to remove the copper hydroxide precipitate to obtain the mother liquor, cool the mother liquor to 10°C, and filter the solid to obtain the crude m-nitrobenzaldehyde, the content of o-nitrobenzaldehyde in the crude m-nitrobenzaldehyde less than 0.5%;

[0025] S3: Put the crude product of m-nitrobenzaldehyde into the reaction device, add ethanol, a water-soluble solvent 3.5 times the v...

Embodiment 3

[0027] S1: Add copper nitrate, water, silver nitrate and catalyst concentrated nitric acid into the reaction device, raise the temperature to 75°C, add benzaldehyde dropwise, the dropwise addition time is 3 hours, continue to heat up to 87°C, and keep warm for 2.5 hours to react. Obtain reaction mixture, wherein the mol ratio of copper nitrate, water, silver nitrate, catalyst concentrated nitric acid and benzaldehyde is 5:40:1:0.2:1; Sampling is carried out chromatographic detection from reaction mixture, and the content of benzaldehyde is less than 0.5 %;

[0028] S2: Filter the reaction mixture to remove the copper hydroxide precipitate to obtain the mother liquor, cool the mother liquor to 15°C, and filter the solid to obtain the crude m-nitrobenzaldehyde, the content of o-nitrobenzaldehyde in the crude m-nitrobenzaldehyde less than 0.5%;

[0029] S3: Put the crude m-nitrobenzaldehyde into the reaction device, add isopropanol, a water-soluble solvent 3.2 times the volume o...

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PUM

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Abstract

The invention relates to the technical field of organic compound synthesis, in particular to a preparation method of benzaldehyde, and aims to improve the product yield, reduce the production cost andreduce environmental damage. The preparation method is characterized by comprising the following steps: S1, adding copper nitrate, water, silver nitrate and catalyst concentrated nitric acid into a reaction device, heating, dropwise adding benzaldehyde, continuously heating, and carrying out heat preservation to react, so as to obtain a reaction mixed solution; and S2, filtering the reaction mixed solution to remove copper hydroxide precipitates to obtain a mother solution, cooling the mother solution, and filtering to obtain a solid m-nitrobenzaldehyde crude product with the content of o-nitrobenzaldehyde less than 0.5%; and S3, putting the m-nitrobenzaldehyde crude product into a reaction device, adding 3.0-3.5 volume times of a water-soluble solvent of that of the m-nitrobenzaldehyde crude product, heating, filtering to remove insoluble impurities, adding water of the same volume of the water-soluble solvent, filtering, taking out precipitated solids, and drying to obtain the high-purity m-nitrobenzaldehyde.

Description

technical field [0001] The invention relates to the technical field of organic compound synthesis, in particular to a preparation method of benzaldehyde. Background technique [0002] m-Nitrobenzaldehyde is a very important pharmaceutical intermediate, which is widely used in the synthesis of various medicines, such as chlorsulone, cilnidipine, nitrendipine, nimodipine, etc. At present, there are very few domestic manufacturers. The reason is that the existing production process is complicated, the selectivity of the ortho-para position is poor, and qualified products need to be recrystallized many times. The high-purity products are not high and the amount of three wastes is large, which is very destructive to the environment. big. Contents of the invention [0003] The object of the present invention is to provide a kind of preparation method of benzaldehyde, aims at improving product yield, reduces production cost, reduces environmental damage. [0004] Above-mentione...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/08C07C205/44
CPCC07C201/08C07C205/44
Inventor 马保方
Owner 枣阳市众成化工有限公司
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