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Synthesis method of bromoacetonitrile

A synthesis method, technology of bromoacetonitrile, applied in chemical instruments and methods, preparation of carboxylic acid nitrile, preparation of organic compounds, etc., can solve problems such as poor safety, high risk, difficult large-scale production, etc., to avoid waste, Ease of transportation and high value utilization

Pending Publication Date: 2021-11-02
宁夏常晟药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This reaction uses bromine as a raw material, and there are high risks in the process of operation, transportation and storage, it is not easy to carry out large-scale production, and the safety is poor

Method used

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  • Synthesis method of bromoacetonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A kind of synthetic method of bromoacetonitrile, this synthetic method comprises:

[0023] (1) Add 600kg of acetone as a solvent in the reaction kettle, then add 400kg of tetramethylammonium bromide, 200kg of chloroacetonitrile, start stirring to dissolve, control the temperature at 70°C, and keep it warm for 4 hours;

[0024] (2) After the reaction, cool down to room temperature, cool down, filter, add the filter residue to 1600kg of methanol, recrystallize and refine to obtain 245.8kg of tetramethylammonium chloride with a purity of 98.6%, rectify the filtrate, and first The solvents acetone and acetonitrile were recovered, and rectification was continued to obtain 283kg of bromoacetonitrile with a purity of 98.9%.

Embodiment 2

[0026] A kind of synthetic method of bromoacetonitrile, this synthetic method comprises:

[0027] (1) Add 600kg of acetone as a solvent in the reaction kettle, then add 500kg of tetramethylammonium bromide, 200kg of chloroacetonitrile, start stirring to dissolve, control the temperature at 70°C, and keep it warm for 4 hours;

[0028] (2) After the reaction, cool down to room temperature, cool down, filter, add the filter residue to 1600kg of methanol, recrystallize and refine to obtain 263.6kg of tetramethylammonium chloride with a purity of 98.9%, rectify the filtrate, and first The solvents acetone and acetonitrile were recovered, and rectification was continued to obtain 291kg of bromoacetonitrile with a purity of 99.3%.

Embodiment 3

[0030] A kind of synthetic method of bromoacetonitrile, this synthetic method comprises:

[0031] (1) Add 600kg of acetone as a solvent in the reaction kettle, then add 700kg of tetramethylammonium bromide, 200kg of chloroacetonitrile, start stirring to dissolve, control the temperature at 70°C, and keep it warm for 4 hours;

[0032] (2) After the reaction, cool down to room temperature, cool down, filter, add the filter residue to 1600kg of methanol, recrystallize and refine to obtain 255.6kg of tetramethylammonium chloride with a purity of 97.8%, carry out rectification of the filtrate, first The solvents acetone and acetonitrile were recovered, and rectification was continued to obtain 285 kg of bromoacetonitrile with a purity of 98.5%.

[0033] In above-mentioned embodiment 1~3, wherein embodiment 2 can be selected as optimal embodiment, at 70 ℃, wherein 300kg acetone, 300kg acetonitrile are as solvent, 500kg tetramethylammonium bromide, 200kg chloroacetonitrile, can obtai...

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Abstract

The invention belongs to the technical field of chemical synthesis, and particularly relates to a synthesis method of bromoacetonitrile. Tetramethylammonium bromide and chloroacetonitrile are used as raw materials and are easy to transport, store and use, and meanwhile, are high in operability in the use process. Meanwhile, in the reaction process, the formed by-product tetramethylammonium chloride exists in a solid form instead of being dissolved in the used solvent and can be directly removed through filtration. Meanwhile, the by-product can be used or sold as a tetramethylammonium chloride product through simple recrystallization treatment and is widely applied to the electronic industry, and high-value utilization is achieved. Besides, the solvent can be recycled through rectification, so that the solvent in the raw material can be reused, the problems of waste of the raw material, environmental pollution and the like are avoided in the process, and an environment-friendly, safe and benefit-maximized production mode and synthesis process of p-bromoacetonitrile are effectively realized.

Description

technical field [0001] The invention belongs to the technical field of compound synthesis, and in particular relates to a synthesis method of bromoacetonitrile. Background technique [0002] Bromoacetonitrile yellow oily liquid. Boiling point: 60-62°C (24mmHg), density (g / mL, 25 / 4°C): 1.93, widely used in the field of organic synthesis. [0003] The method of the synthetic bromoacetonitrile of report both at home and abroad has: [0004] Japanese Patent JP5359799A: Based on acetonitrile, in the absence of solvent, hydrogen chloride gas is blown into the acetonitrile reaction system, and bromine is dripped into the system under light irradiation. For example, a 100w high-pressure mercury lamp emits ultraviolet rays with a wavelength of 3650-3690 A. The reaction conditions of this reaction are strictly controlled, and the equipment is relatively complicated. [0005] Japanese Patent JP20454987A: By brominating acetonitrile with bromine in the presence of phosphorus tribromi...

Claims

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Application Information

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IPC IPC(8): C07C253/30C07C255/10
CPCC07C253/30C07C255/10
Inventor 陈健龙刘超
Owner 宁夏常晟药业有限公司
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