Method for continuously preparing benzyl bromide derivative

A technology for benzyl bromide derivatives and derivatives, which is applied in the field of continuous preparation of benzyl bromide derivatives, can solve the problems of dibromine by-products, troublesome separation and processing, and achieves the advantages of optimizing reaction conditions, improving selectivity and reducing production costs. Effect

Pending Publication Date: 2022-07-22
浙江禾本科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] As mentioned above, the current preparation of benzyl bromide derivatives by reacting toluene derivatives with brominating agents is basically carried out in batch operation reactors, which has the disadvantages of easily generating dibromo by-products and troublesome subsequent separation and treatment.

Method used

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  • Method for continuously preparing benzyl bromide derivative
  • Method for continuously preparing benzyl bromide derivative
  • Method for continuously preparing benzyl bromide derivative

Examples

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Effect test

Embodiment 1

[0026] This embodiment provides a method for preparing 2-nitrobenzyl bromide by continuous reaction. The reaction is carried out in a continuously operating fully mixed flow reactor, the reactor is specifically a 5L glass stirred tank reactor, and the reaction materials are the solvent PhCl, The toluene derivative is 2-nitrotoluene, the initiator is AIBN, the brominating agent is 48% HBr, and the concentration of H is 50%. 2 O 2 .

[0027] The specific steps are:

[0028] 101. In the reaction, the material is put into the reactor according to a certain flow rate. The flow rate of the material is: the flow rate of the solvent PhCl is 685g / h, the flow rate of 2-nitrotoluene is 137g / h, the flow rate of the initiator AIBN is 2.75g / h, and the flow rate of 48% HBr 112.5g / h, 50%H 2 O 2 The flow rate was 45.3 g / h, and the mixture was formed at 80 °C;

[0029] 102, washing and stratification, the reaction mixture leaving the fully mixed flow reactor continuously enters the washing...

Embodiment 2

[0036] This embodiment provides a method for preparing 2-nitrobenzyl bromide by continuous reaction. The reaction is carried out in a continuously operating fully mixed flow reactor, the reactor is specifically a 5L glass stirred tank reactor, and the reaction materials are the solvent PhCl, 2-nitrotoluene, initiator AIBN, bromine (Br 2 ), 50%H 2 O 2 .

[0037] The specific steps are:

[0038] 201. Reaction, the material is put into the reactor according to a certain flow rate, and the material flow rate is: the flow rate of the solvent PhCl is 685g / h, the flow rate of 2-nitrotoluene is 137g / h, the flow rate of the initiator AIBN is 2.75g / h, the flow rate of bromine (Br 2 ) flow rate is 53.5g / h, 50%H 2 O 2 The flow rate was 22.7 g / h, and the mixture was formed at a temperature of 80 °C;

[0039] 202, washing and stratifying, the reaction mixture leaving the fully mixed flow reactor continuously enters the washing stratifying device, adds water, and allows to stand after ...

Embodiment 3

[0043] This embodiment provides a method for preparing 2-cyanobenzyl bromide by continuous reaction. The reaction is carried out in a continuously operating fully mixed flow reactor, the reactor is specifically a 5L glass stirred tank reactor, and the reaction materials are solvent EDC, 2-cyanotoluene, initiator AIBN, 48%HBr, 50%H 2 O 2 .

[0044] The specific steps are:

[0045] 301. The material is put into the reactor according to a certain flow rate. The flow rate of the material is: the flow rate of the solvent EDC is 685g / h, the flow rate of 2-cyanotoluene is 137g / h, the flow rate of the initiator AIBN is 2.75g / h, and the flow rate of 48% HBr is 130g / h, 50%H 2 O 2 The flow rate was 52.3 g / h, and the mixture was formed at a temperature of 70 °C;

[0046] 302, washing and stratification, the reaction mixture leaving the fully mixed flow reactor enters the washing stratification device continuously, adds water, and after mixing, it is left to stand, and the water phas...

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Abstract

The invention discloses a method for continuously preparing benzyl bromide derivatives, and particularly relates to the field of chemical production, the method comprises four parts of reaction, washing and layering, desolvation and separation, reaction materials comprise a solvent, toluene derivatives, an initiator, a brominating agent, hydrogen peroxide and the like, and the method comprises the following specific steps: adding the reaction materials into a reactor according to a certain flow rate; the material flow rates are as follows: the flow rate of a solvent PhCl is 685 g / h, the flow rate of 2-nitrotoluene is 137 g / h, the flow rate of an initiator AIBN is 2.75 g / h, the flow rate of 48% HBr is 112.5 g / h, the flow rate of 50% H2O2 is 45.3 g / h, and a mixture is generated at the temperature of 80 DEG C; washing and layering, continuously feeding a reaction mixture leaving the complete mixing flow reactor into a washing and layering device, discharging a water phase and an organic phase, discharging the water phase, and feeding the organic phase into a desolventizing kettle; desolventizing: desolventizing an organic phase generated by washing and layering to obtain a solvent PhCl, and recycling the solvent PhCl; separating, desolventizing, feeding into a separator, separating and recovering the obtained 2-nitrotoluene by the separator, and returning to the complete mixing flow reactor for complete mixing flow.

Description

Technical field [0001] The present invention relates to the technical field of chemical production, and more specifically, the present invention relates to a method for continuously preparing benzyl bromide derivatives. Background technique [0002] Benzyl bromide derivatives are important organic chemical intermediates and have important applications in drug synthesis. For example, 2-nitrobenzyl bromide can be used to synthesize the fungicide Pyraclostrobin, 2-cyanobenzyl Bromine can be used as an organic synthesis intermediate and pharmaceutical intermediate, and can be used in laboratory research and development processes and chemical production processes. (E)-α-Methoxyimino-2-(bromomethyl)phenylacetic acid methyl ester can be used Synthetic fungicide trifloxystrobin. [0003] At present, one of the main synthesis methods of benzyl bromide derivatives is to react toluene derivatives with brominating agents in solvents under initiator or light conditions. The above-menti...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C07C205/11C07C201/12C07C255/50C07C253/30C07C251/48C07C249/12
CPCC07C201/12C07C253/30C07C249/12C07C205/11C07C255/50C07C251/48
Inventor王进廖道华潘光飞童圆圆綦菲廖文斌曾挺
Owner浙江禾本科技股份有限公司