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Synthesis process of 5-nitro-2-(3-nitrophenyl) benzimidazole

A synthesis process, a nitrophenyl technology, applied in directions such as organic chemistry, can solve problems such as difficult industrial production, difficult temperature control, serious environmental pollution, etc., and achieve the effects of improving purity, simple and convenient synthesis, and reducing production costs.

Pending Publication Date: 2022-04-15
天津众泰材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] 1) Using 4-nitro-o-phenylenediamine and 3-nitrobenzaldehyde as reaction raw materials, condensing 5-nitro-2-(3-nitrophenyl) benzimidazole through hydrochloric acid and hydrogen peroxide system, this method When hydrogen peroxide is used, it is difficult to control the temperature in the system during scale-up, and the safety factor is low. At the same time, the waste liquid contains a large amount of acid water and hydrogen peroxide ， The three wastes are troublesome to deal with, the environment is seriously polluted, and it is difficult to realize industrial production;
[0004] 2) Also take 4-nitro-o-phenylenediamine and 3-nitrobenzaldehyde as reaction raw materials, synthesize 5-nitro-2-(3-nitrophenyl) benzimidazole through zinc oxide and hydrogen peroxide system, because The hydrogen peroxide in the system, so the same problem, the reaction cannot be controlled during the scale-up production, the safety risk is high, and a large amount of waste solids and waste liquid containing hydrogen peroxide are produced by the reaction at the same time, and the treatment of the three wastes is difficult

Method used

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  • Synthesis process of 5-nitro-2-(3-nitrophenyl) benzimidazole

Examples

Experimental program
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Effect test

Embodiment 1

[0026] In the present embodiment, the synthetic method of 5-nitro-2-(3-nitrophenyl) benzimidazole comprises the following steps:

[0027] (1) raw material selection, with 4-nitro o-phenylenediamine and 3-nitrobenzaldehyde as reaction raw materials. For selection (EtOH / H 2 O,Na 2 S 2 o 5 ) as a reaction system;

[0028] (2) To synthesize an intermediate, add 10V ethanol (3L) to the reaction flask at room temperature, start stirring, and continue to add 1.1eq of 3-nitrobenzaldehyde (325g) to the system, 10V purified water (3L), 1.1eq Sodium metabisulfite (409.4g), stirred at room temperature for 1h;

[0029] (3) Synthesize the crude product, add 1.0eq of 4-nitro-o-phenylenediamine (300g) to the system, turn on the heating, control the internal temperature at 75°C-80°C, stir the reaction for 46h, monitor the liquid phase (4-nitro-o-phenylenediamine O-phenylenediamine ≤ 3%), 10V purified water (3L) was added dropwise to the system, after the dropwise addition was completed, ...

Embodiment 2

[0035] In the present embodiment, the synthetic method of 5-nitro-2-(3-nitrophenyl) benzimidazole comprises the following steps:

[0036] (1) raw material selection, with 4-nitro o-phenylenediamine and 3-nitrobenzaldehyde as reaction raw materials. For selection (EtOH / H 2 O,Na 2 S 2 o 5 ) as a reaction system;

[0037] (2) To synthesize an intermediate, add 10V ethanol (3L) to the reaction flask at room temperature, start stirring, and continue to add 1.1eq of 3-nitrobenzaldehyde (325g), 10V purified water (3L), 2eq of Sodium metabisulfite (744g), stirred and reacted at room temperature for 1h;

[0038] (3) Synthesize the crude product, add 1.0eq of 4-nitro-o-phenylenediamine (300g) to the system, turn on the heating, control the internal temperature at 75°C-80°C, stir the reaction for 46h, monitor the liquid phase (4-nitro-o-phenylenediamine O-phenylenediamine ≤ 3%), 10V purified water (3L) was added dropwise to the system, after the dropwise addition was completed, the...

Embodiment 3

[0041] In the present embodiment, the synthetic method of 5-nitro-2-(3-nitrophenyl) benzimidazole comprises the following steps:

[0042] (1) raw material selection, with 4-nitro o-phenylenediamine and 3-nitrobenzaldehyde as reaction raw materials. For selection (EtOH / H 2 O,Na 2 S 2 o 5 ) as a reaction system;

[0043] (2) To synthesize an intermediate, add 10V ethanol (3L) to the reaction flask at room temperature, start stirring, and continue to add 1.1eq of 3-nitrobenzaldehyde (325g) to the system, 10V purified water (3L), 1.1eq Sodium metabisulfite (409.4g), stirred at room temperature for 1h;

[0044] (3) Synthesize the crude product, add 1.0eq of 4-nitro-o-phenylenediamine (300g) to the system, turn on the heating, control the internal temperature at 75°C-80°C, stir the reaction for 46h, monitor the liquid phase (4-nitro-o-phenylenediamine O-phenylenediamine ≤ 3%), 10V purified water (3L) was added dropwise to the system, after the dropwise addition was completed, ...

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Abstract

The invention provides a synthesis process of 5-nitro-2-(3-nitrophenyl) benzimidazole, which comprises the following steps: stirring sodium pyrosulfite, purified water, a solvent and 3-nitrobenzaldehyde at room temperature for reaction to obtain a first reaction solution; 4-nitro-o-phenylenediamine is added into the first reaction liquid, heating and stirring are carried out, purified water is dropwise added, cooling and suction filtration are carried out, and a crude product is obtained; and mixing the crude product, an alkali solution and absolute ethyl alcohol until the mixture is completely dissolved, dropwise adding concentrated hydrochloric acid, filtering, purifying and washing solids, and carrying out vacuum drying to obtain the required product. The synthesis process of the 5-nitro-2-(3-nitrophenyl) benzimidazole is simple and convenient in synthesis, can improve the yield and purity of the 5-nitro-2-(3-nitrophenyl) benzimidazole, and can be applied to industrial production.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a synthesis process of 5-nitro-2-(3-nitrophenyl)benzimidazole. Background technique [0002] Synthetic 5-nitro-2-(3-nitrophenyl) benzimidazole main literature report has two kinds of methods at present: [0003] 1) Using 4-nitro-o-phenylenediamine and 3-nitrobenzaldehyde as reaction raw materials, condensing 5-nitro-2-(3-nitrophenyl) benzimidazole through hydrochloric acid and hydrogen peroxide system, this method When hydrogen peroxide is used, it is difficult to control the temperature in the system during scale-up, and the safety factor is low. At the same time, the waste liquid contains a large amount of acid water and hydrogen peroxide ， The three wastes are troublesome to deal with, the environment is seriously polluted, and it is difficult to realize industrial production; [0004] 2) Also take 4-nitro-o-phenylenediamine and 3-nitrobenzaldehyde as reaction raw materials,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D235/18
Inventor 栗晓东
Owner 天津众泰材料科技有限公司
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