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Preparation method of 2-nitrobenzyl bromide

A technology of nitrobenzyl bromide and o-nitrotoluene, applied in the field of chemical synthesis, can solve the problems of shortened reaction time, low product yield and purity, long reaction cycle and the like, and achieves shortened reaction time, fast reaction speed and easy operation. Effect

Active Publication Date: 2018-08-24
HEBEI CHENGXIN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Aiming at the problems of long reaction period, low product yield and low purity in the synthesis process of o-nitrobenzyl bromide, the present invention designs a preparation method of o-nitrobenzyl bromide, that is, provides a method that can make o-nitrobenzyl bromide, hydrogen bromide Acid and hydrogen peroxide react completely in a microchannel reactor, reducing operating procedures, greatly shortening reaction time, and further improving the purity and yield of the target product o-nitrobenzyl bromide. This method has no obvious "magnification effect", Suitable for industrial mass production

Method used

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  • Preparation method of 2-nitrobenzyl bromide

Examples

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Embodiment 1

[0039] 1) After the mass percentage of 99.15% o-nitrotoluene and azobisisobutyronitrile are mixed and dissolved, pass into the first module through a metering pump with a mass flow of 7g / min, and azobisisobutyronitrile is 0.03 of the mass of o-nitrotoluene;

[0040] 2) with the mass percentage composition of 5% hydrogen peroxide solution, the mass flow of 24g / min is passed into the first module and mixed with o-nitrotoluene and azobisisobutyronitrile mixed solution, and the o-nitro The molar ratio of toluene and hydrogen peroxide is 1.00:0.7, and the first module controls the reaction temperature to be 60°C;

[0041] 3) The mixed feed liquid that step 1) and step 2) are processed are pumped into the second module, and synchronously the mass percentage of 5% hydrobromic acid is passed into the second module with a mass flow of 50g / min through a metering pump , carry out mixing and reaction, the second module controls the reaction temperature to be 150°C, and the molar ratio of...

Embodiment 2

[0046] 1) after the mass percentage composition is 99.56% o-nitrotoluene and benzoyl peroxide mixed and dissolved, pass into the first module through a metering pump with the mass flow of 15g / min, and benzoyl peroxide is an o-nitroxide. 0.08 of the mass of toluene;

[0047] 2) with the mass percentage composition of 30% hydrogen peroxide solution, pass into the first module with the mass flow of 15g / min and mix with o-nitrotoluene and benzoyl peroxide mixed solution, o-nitrotoluene The molar ratio with hydrogen peroxide is 1.00:1.2, and the first module controls the reaction temperature to be 70°C;

[0048]3) The mixed feed liquid processed in step 1) and step 2) is pumped into the second module, and the hydrobromic acid that the mass percentage is 48% is passed into the second module with the mass flow of 20g / min through the metering pump synchronously. , carry out mixing and reaction, the second module controls the reaction temperature to be 110°C, and the molar ratio of o-...

Embodiment 3

[0053] 1) after 99.87% o-nitrotoluene and cumene hydrogen peroxide are mixed and dissolved by mass percentage, pass into the first module through a metering pump with the mass flow of 11g / min, and cumene hydrogen peroxide is 0.05 of the mass of o-nitrotoluene;

[0054] 2) be the hydrogen peroxide solution of 20% by mass percentage, pass into the first module with the mass flow rate of 14g / min and mix with o-nitrotoluene and cumene hydrogen peroxide mixed solution, o-nitrotoluene and cumene hydrogen peroxide mixed solution. The molar ratio of toluene and hydrogen peroxide is 1.00:1.0, and the first module controls the reaction temperature to be 65°C;

[0055] 3) The mixed feed liquid processed in step 1) and step 2) is pumped into the second module, and the hydrobromic acid that the mass percentage is 20% is passed into the second module with the mass flow of 26g / min through the metering pump synchronously. , carry out mixing and reaction, the second module controls the reacti...

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Abstract

The invention discloses a preparation method of 2-nitrobenzyl bromide, and belongs to the technical field of chemical synthesis. According to the method, o-nitrotoluene, hydrobromic acid and hydrogenperoxide are taken as raw materials, under the initiation of catalysts, the 2-nitrobenzyl bromide is generated by conducting substitution reaction through a micro-channel reactor constantly; the 2-nitrobenzyl bromide is prepared through the micro-channel reactor, the operation is simple, the procedures are simple and the reaction time is greatly shortened.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and relates to a preparation method for preparing o-nitrobenzyl bromide. The invention utilizes a microchannel reactor to prepare the o-nitrobenzyl bromide, has simple operation, simple procedure and greatly shortens the reaction time. Background technique [0002] Pyraclostrobin is a new type of bactericide of methoxyacrylate, which is a new broad-spectrum bactericide. Its mechanism of action is a mitochondrial respiration inhibitor, which prevents mitochondria from producing and providing the energy required for normal cell metabolism, and eventually leads to cell death. die. In addition to its excellent bactericidal properties, pyraclostrobin can promote the absorption of nitrogen by crops and stimulate faster growth of plants. With the increasing demand for pyraclostrobin in recent years, more and more studies have been conducted on the yield of its intermediates. [0003] Ortho...

Claims

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Application Information

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IPC IPC(8): C07C205/11C07C201/12
CPCC07C201/12C07C205/11
Inventor 刘少华董璞祝兆军李建乐张艳章李晓俊
Owner HEBEI CHENGXIN
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