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Method for preparing 2,2-dibromo-3-cyanoacetamide

A technology of cyanoacetamide and cyanoacetamide is applied in the preparation of carboxylic acid nitrile, chemical instruments and methods, preparation of organic compounds, etc., and can solve the problems of production safety, increase in impurities, complicated processes, etc. The effect of reducing factory costs

Inactive Publication Date: 2010-02-17
中国中化股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to solve the above-mentioned preparation method adopt H 2 o 2 Problems such as production safety, impurity increase, cost increase, and complicated process brought by the oxidant, the invention provides a new method for preparing 2,2-dibromo-3-cyanoacetamide
This method utilizes industrial alkali bromide mother liquor as bromine source for the first time, adopts chlorine gas as oxidant, fundamentally solves the 2 o 2 many problems brought as oxidizing agent, thereby completed the present invention

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0020] Add 10g of cyanoacetamide, 25g of NaBr, and 50ml of water into the reaction flask. Stir to dissolve, then introduce chlorine gas through the bottom tube, and control the rate of introducing chlorine gas to about 3L / h. The temperature rises naturally, and the temperature is controlled at 60-80°C. After 1 hour of reaction, 10 g of chlorine gas was introduced, and the temperature in the reaction flask was no longer raised, and the chlorine gas flow was stopped. Detect the pH of the reaction solution in the kettle to be 4, and continue to insulate and stir for 30 minutes. Then it was cooled with ice water until the white crystalline product precipitated. After suction filtration and drying, 27.4 g of 2,2-dibromo-3-cyanopropionamide was obtained, with a yield of 95% based on cyanoacetamide and a liquid chromatography analysis content of 99.5%.

example 2

[0022] Be that 30% NaBr mother liquor replace the reagent NaBr among the example 1 with 84g content. Other feeding and operating conditions are with example 1. 27 g of 2,2-dibromo-3-cyanopropionamide was obtained, with a yield of 94% and a content of 99.5%.

example 3

[0024] Weigh 10 g of cyanoacetamide into a four-neck flask, add 84 g of 30% NaBr mother liquor to dissolve. Chlorine gas is introduced through the bottom pipe, and the rate of chlorine gas introduction is controlled to be about 4L / h. The temperature rises naturally, and the temperature is controlled at 30-50°C. The reaction time was 58 minutes, the chlorine gas flow rate was 12.5 g, and the temperature was no longer raised, so the chlorine gas flow was stopped. The pH of the reaction solution in the test kettle was detected to be 3, and the temperature was continued for 30 minutes. Afterwards, the operation was the same as in Example 1 to obtain 26.8 g of 2,2-dibromo-3-cyanopropionamide, with a yield of 93% and a content of 99.5%.

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PUM

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Abstract

The invention discloses a method for preparing 2,2-dibromo-3-cyanoacetamide, comprising the following steps: taking cyanoacetamide and industrial bromide alkali liquor as raw materials; and directingintroducing chlorine to a water medium for oxidative bromination reaction. The reaction temperature is 10 to 80 DEG C. The mole number for feeding comprises: alkali bromide is 2.0 to 2.5 times of thecyanoacetamide, and the chlorine is 0.55 to 0.7 times of the alkali bromide. The invention has the advantages of simple process, mild operating condition and easy control, takes full advantage of theindustrial bromide alkali liquor and greatly reduces the production cost of factories.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a method for preparing 2,2-dibromo-3-cyanoacetamide. Background technique [0002] 2,2-Dibromo-3-cyanopropionamide (DBNPA for short) is a new type of high-efficiency disinfectant and excellent water treatment agent, and is an ideal environment-friendly sterilization product. The traditional production process of 2,2-dibromo-3-cyanopropionamide at home and abroad uses cyanoacetamide as raw material to react with bromine to generate 2,2-dibromo-3-cyanoacetamide, and at the same time Hydrogen bromide is produced, and this process (referred to as the full bromine method) has the disadvantage of low bromine utilization rate. EP 308184A discloses a 2 o 2 As an oxidizing agent, the hydrogen bromide generated in the reaction is oxidized to bromine again, and the perbromine method is improved to achieve the purpose of improving the utilization rate of bromine. Korean patent KR185280B1...

Claims

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Application Information

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IPC IPC(8): C07C255/19C07C253/30
Inventor 李付刚李文骁闫士杰白雪松
Owner 中国中化股份有限公司
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