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Method for preparing 2-amino-5-bromo-N,3-dimethyl-benzamide

A technology of dimethylbenzamide and amino group, which is applied in electrolytic components, electrolytic organic production, electrolytic process and other directions, can solve the problems of long reaction time of synthesis process, corrosive environment of equipment and high production cost, and achieves good product purity and high yield. The effect of high rate and short reaction time

Inactive Publication Date: 2013-04-24
HARBIN UNIV OF SCI & TECH
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  • Application Information

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Problems solved by technology

[0006] The present invention provides a 2-amino-5-bromo-N,3-dimethylbenzamide synthesis process for solving the problems of long reaction time, high production cost, equipment corrosion and environmental pollution. -5-bromo-N, the preparation method of 3-dimethylbenzamide

Method used

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  • Method for preparing 2-amino-5-bromo-N,3-dimethyl-benzamide

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specific Embodiment approach 1

[0015] Specific embodiment 1: A preparation method of 2-amino-5-bromo-N,3-dimethylbenzamide in this embodiment is carried out according to the following steps:

[0016] 1. Weigh out 2-amino-N,3-dimethylbenzamide according to the mass ratio of 2-amino-N,3-dimethylbenzamide and hydrobromic acid solution at 1:(1~3) And hydrobromic acid solution, and then press the volume ratio of 2-amino-N,3-dimethylbenzamide to tetrahydrofuran as 1g: (5-10) mL, press 2-amino-N,3-dimethyl The mass ratio of benzamide to the volume of dilute sulfuric acid is 1g: (8-14) mL, and tetrahydrofuran and dilute sulfuric acid are weighed; the mass concentration of hydrobromic acid solution is 35% to 45%, and the mass concentration of dilute sulfuric acid is 10%~20%;

[0017] 2. In a single-chamber non-diaphragm electrolytic cell, the metal platinum sheet is used as the cathode and anode electrodes, and the distance between the electrodes is 0.5 to 1.5 cm. The 2-amino-N,3-weighed in step 1 is sequentially added ...

specific Embodiment approach 2

[0020] Specific embodiment two: This embodiment is different from specific embodiment one in that the mass ratio of 2-amino-N,3-dimethylbenzamide and hydrobromic acid solution in step one is 1:2, and other steps are The parameters are the same as in the first embodiment.

specific Embodiment approach 3

[0021] Specific embodiment three: This embodiment is different from specific embodiment one or two in that the mass concentration of the hydrobromic acid solution in step one is 40%, and other steps and parameters are the same as those in specific embodiment one or two.

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Abstract

The invention relates to a method for preparing 2-amino-5-bromo-N,3-dimethyl-benzamide. For solving the problems of the existing 2-amino-5-bromo-N,3-dimethyl-benzamide synthetic process, such as long reaction time, high production cost, corrosion of equipment and environmental pollution, the preparation method comprises the following steps: in a single-room electrolytic tank without diaphragms, adopting metal platinum sheets as anodic and cathodic electrodes, adopting dilute sulphuric acid and hydrobromic acid liquor as electrolyte, and adopting 2-amino-bromo-N,3-dimethyl-benzamide as raw material; reacting and synthesizing 2-amino-5-bromo-N,3-dimethyl-benzamide in a slightly alkaline system; and adopting the hydrobromic acid to carry out the bromination reaction. The method can prevent the equipment corrosion and environmental pollution caused by the liquid bromine, has a high product yield which achieves 97.12% and a high purity which achieves 95%, and has the performances of gentle reaction conditions, short reaction time and low energy consumption, so that the method is suitable for industrial production.

Description

Technical field [0001] The invention relates to a preparation method of 2-amino-5-bromo-N,3-dimethylbenzamide. Background technique [0002] 2-Amino-5-bromo-N,3-dimethylbenzamide is an important intermediate for the synthesis of cyantraniliprole, an o-carboxamidobenzamide insecticide. At present, there are mainly three synthetic methods reported in the literature for 2-amino-5-bromo-N,3-dimethylbenzamide, which are as follows: [0003] (1) Using 2-amino-N,3-dimethylbenzamide as raw material, glacial acetic acid as solvent, sodium hydroxide solution and liquid bromine as brominating reagents, the reaction system is at 45℃ under nitrogen protection After reacting for more than 15 hours, 2-amino-5-bromo-N,3-dimethylbenzamide is obtained. The yield was 89.7%. The main disadvantage of this method is that strong corrosive liquid bromine is used in the reaction process, which requires high reaction equipment, and the reaction time is too long, which is not conducive to industrial produ...

Claims

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Application Information

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IPC IPC(8): C25B3/06
Inventor 张娟由君刘波喻艳超
Owner HARBIN UNIV OF SCI & TECH
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