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Preparation method of bromoacetonitrile

A technology of bromoacetonitrile and chloroacetonitrile, applied in the synthesis field of bromoacetonitrile, can solve the problems of high price, high risk, poor safety, etc., and achieve the effects of less waste discharge, green process route, and easy operation.

Pending Publication Date: 2022-07-22
上海巽田科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It avoids the disadvantages of bromine as a raw material, high risk in the process of operation, transportation and storage, and it is not easy to carry out large-scale production and poor safety.
However, tetramethylammonium bromide is not easy to obtain and the price is high, so the process is not competitive in cost

Method used

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  • Preparation method of bromoacetonitrile
  • Preparation method of bromoacetonitrile
  • Preparation method of bromoacetonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (1) In a 5L four-necked flask, add methanol 2.1Kg, chloroacetonitrile 1.0Kg, catalyst [Prmim]Cl 2.1g (0.1mol%), then add sodium bromide 1.5Kg (1.1eq), stir rapidly, and heat up to 75 The reaction was carried out at °C for 10 hours. After the reaction was completed, GC was tested, the conversion rate was 98.1%, and the selectivity was 99.1%.

[0044] (2) reaction system is lowered to room temperature, filtered, washed filter cake with methanol 200g, the filtrate was merged, and methanol was recovered by atmospheric distillation for subsequent reaction, and the heavy component was subjected to vacuum distillation to obtain 1.44Kg of bromoacetonitrile, yield 90.6%, purity 99.2%. The catalyst remaining at the bottom of the rectification tank is recovered and applied mechanically.

Embodiment 2

[0046] The target product bromoacetonitrile was prepared according to the same method as in Example 1, except that the catalyst in step (1) was [Prmim]Br.

Embodiment 3

[0048] The target product bromoacetonitrile was prepared according to the same method as in Example 1, except that the catalyst in step (1) was [Memim]Br.

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PUM

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Abstract

The invention discloses a bromoacetonitrile preparation method, which comprises: 1) adding chloroacetonitrile, a bromine salt, a catalyst and a solvent to a reactor, and carrying out a reaction at a certain temperature; and 2) after the reaction is finished, cooling the reaction system to room temperature, filtering, washing a filter cake with a small amount of solvent, combining filtrate, distilling the filtrate to recover the solvent, then carrying out reduced pressure rectification on the residual heavy component after the solvent is recovered to obtain the target product bromoacetonitrile, and recovering and reusing the residual catalyst at the bottom of a rectifying still. According to the method disclosed by the invention, chloroacetonitrile and bromine salt are used as raw materials, and bromoacetonitrile is obtained with high yield under mild conditions in the presence of the catalyst. Compared with other routes, the used raw materials are safer and cheaper, and the used process is convenient to operate, free of acid gas and free of corrosion; the obtained product is high in purity and lower in cost. The catalyst used in the process can be recycled, so that the emission of wastes is greatly reduced, and the process route is greener.

Description

technical field [0001] The invention belongs to the field of organic chemical industry, and in particular relates to a method for synthesizing bromoacetonitrile. Background technique [0002] Bromoacetonitrile is a yellow oily or light amber liquid with a boiling point of 150-151°C (100kPa) and a relative density of 1.722. It is soluble in ether and slightly soluble in ethanol. Widely used in the fields of medicine and fine chemicals. [0003] The traditional synthesis method of bromoacetonitrile is through the bromination reaction of acetonitrile and bromine. Japanese patent JP2000247941A reported that in the presence of hydrochloric acid gas, acetonitrile was brominated with bromine under the irradiation of light to prepare bromoacetonitrile. Japanese patent JP2517304B2 has reported that in the presence of phosphorus tribromide, acetonitrile and bromine carry out bromination reaction to produce the process of bromoacetonitrile. In addition, there are also reports that a...

Claims

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Application Information

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IPC IPC(8): C07C253/30C07C255/10
CPCC07C253/30C07C255/10
Inventor 张少春刘晓然王喜成林世清牟新东
Owner 上海巽田科技股份有限公司
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