Synthetic method of 2-cyanogroup-4-nitro-6-bromaniline diazosalt

A synthesis method and technology for p-nitroaniline are applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., and can solve problems such as insufficient operation, large floor space, complicated processes, etc., and achieve shortening of production processes, The effect of less three wastes and simple process

Active Publication Date: 2010-03-17
HANGZHOU JIHUA JIANGDONG CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are disadvantages such as cumbersome process, not easy to operate, large floor are

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0019] Example 1

[0020] Add 200 g of sulfuric acid with a mass percentage of 60% into the flask, add 32.6 g of p-nitroaniline with zirconium cyanide under stirring, and heat up to 50° C. to maintain. The dropwise addition of 18.2 g of bromine was started, and the reaction temperature was 20-25°C. After holding, 13.1 g of 30% hydrogen peroxide was added dropwise, and the dropwise temperature was controlled at 20-25°C. End-point sampling analysis, the main content is 97.52%, and the raw material is 0.77%;

[0021] 70 g of 40% nitrosyl sulfuric acid was added dropwise at a temperature of 10-15° C. for diazotization, and kept for 3.0 hours after the dropwise addition. The diazonium salt is coupled by conventional methods to obtain Disperse Blue 183:1 dye. 86.3 g of dry dye was obtained, with excellent dye performance and 92.8% dye chromatographic content.

Example Embodiment

[0022] Example 2

[0023] 500 g of sulfuric acid with a mass percentage of 30% was added to the flask, and 32.6 g of pyrimethacrylate-p-nitroaniline was added under stirring, and the temperature was raised to 40°C. Then 23.7g of sodium bromide was added, and the temperature of the addition was controlled at 40°C. After holding, 13.5 g of hydrogen peroxide was added dropwise, and the dropwise temperature was controlled at 45-50°C. Sampling and analysis after the end point, the main content is 97.2%, and the raw material is 0.4%;

[0024] At this temperature, 72 g of 40% nitrosyl sulfuric acid was added dropwise for diazotization, and the solution was kept for 3.0 hours after the dropwise addition. The diazonium salt is coupled by conventional methods to obtain Disperse Blue 183:1 dye. 87.0g of dry dye products were obtained. Dye performance is excellent. Dye chromatographic content 92.6%.

Example Embodiment

[0025] Example 3

[0026] 400 g of sulfuric acid with a mass percentage of 40% was added to the flask, and 32.6 g of bis-cyano-p-nitroaniline was added under stirring, and the temperature was raised to 30°C. Then 23.7g of sodium bromide was added, and the temperature of the addition was controlled at 30°C. After holding, 17 g of chlorine gas was introduced, and the temperature was controlled at 30 °C. Sampling and analysis after the end point, the main content is 97.5%, and the raw material is 0.5%;

[0027] At this temperature, 72 g of 40% nitrosyl sulfuric acid was added dropwise for diazotization, and the solution was kept for 3.0 hours after the dropwise addition. The diazonium salt is coupled by conventional methods to obtain Disperse Blue 183:1 dye. 86.5g of dry dye was obtained, with excellent dye performance. Dye chromatographic content 91.76%.

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PUM

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Abstract

The invention relates to a synthetic method of 2-cyanogroup-4-nitro-6-bromaniline diazosalt, solving the technical problems of simple technique and operation, low requirement for production field andequipment, and low energy consumption and low 'three wastes'. The invention comprises the following steps: using o-cyanogroup paranitroaniline as a raw material, pulping in the sulphuric acid at the mass percent of 10% to 98%, adding brominated compound and oxidant for bromination, and directly diazotizing the mixture with the diazotized agent after bromination to obtain the product, wherein the molar ratio of o-cyano paranitroaniline sulphuric acid, brominated compound, oxidant and diazotized agent is 1:3.0 to 20.0:0.5 to 1.5:0.4 to 1.5:1.0 to 2.0.

Description

technical field [0001] The invention relates to a preparation method of an organic compound, in particular to a synthesis method of 2-cyano-4-nitro-6-bromoaniline diazonium salt. technical background [0002] 2-cyano-4-nitro-6-bromoaniline is an important dye intermediate, and the commonly used process is o-cyano-p-nitroaniline in hydrochloric acid medium, brominated with bromine, and then chlorine or Sodium chlorate replaces bromine in the reaction system and further brominates, and then obtains solid 2-cyano-4-nitro-6-bromoaniline through filtration, washing and drying; the obtained solid 2-cyano-4-nitro Base-6-bromoaniline is then reacted with diazotization reagents such as sulfuric acid and nitrosyl sulfuric acid or nitrite to obtain diazonium salt. There are disadvantages such as cumbersome process, inconvenient operation, large area required for production, more equipment, high energy consumption and more three wastes. Contents of the invention [0003] The technic...

Claims

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Application Information

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IPC IPC(8): C07C255/65C07C253/30
Inventor 简卫陈美芬陆洪汇
Owner HANGZHOU JIHUA JIANGDONG CHEMICAL CO LTD
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