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Synthesis method of 2,4-dichloro-5-isopropoxy aniline

A technology of propoxyaniline and a synthesis method, applied in 2 fields, can solve the problems of cumbersome process operation, large amount of three wastes, poor product quality, etc., and achieves the effects of reducing production cost, improving yield, and improving product quality

Active Publication Date: 2010-09-08
ANHUI KELIHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are many ways to realize this process, but the method that has been widely used for a long time is the iron powder reduction method. The iron powder reduction method has the advantages of good selectivity and low synthesis cost, but this method also has a large amount of "three wastes". The process operation is cumbersome, the synthesis yield is low, and the product quality is poor.

Method used

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  • Synthesis method of 2,4-dichloro-5-isopropoxy aniline
  • Synthesis method of 2,4-dichloro-5-isopropoxy aniline
  • Synthesis method of 2,4-dichloro-5-isopropoxy aniline

Examples

Experimental program
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Effect test

Embodiment 1

[0025] With 2,4-dichlorophenol as the starting material, 100g of 2,4-dichloro-5-isopropoxynitrobenzene (content 91.6% ) into the four-necked bottle, which is respectively equipped with a thermometer, an electric stirring device, a condenser and a constant pressure funnel, and the 150mL specification is 95% (V / V) ethanol and 20g composite catalyst {10g gac, 5g Fe(OH) 3 , 5g Al(OH) 3} into the four-necked flask, stirred for 0.5 hours, and began to heat. When the temperature rose to 65°C, 45.8g of hydrazine hydrate (80%) was slowly dripped into the four-necked flask from the constant pressure funnel, and the dropping time was 1 ~3 hours, continue to react at 60~80°C for 2~6 hours after dropping, stop the reaction, cool down to 30°C, and obtain the filtrate by suction filtration, which is 2,4-dichloro-5-isopropoxyaniline solution . The weight of the filtrate was 254.5 g, the content of 2,4-dichloro-5-isopropoxyaniline in the filtrate was 30.5%, and the reaction yield was 96.3%....

Embodiment 2

[0027] With 2,4-dichlorophenol as the starting material, 100g of 2,4-dichloro-5-isopropoxynitrobenzene (content 91.6% ) into the four-necked bottle, which is respectively equipped with a thermometer, an electric stirring device, a condenser and a constant pressure funnel, and the 150mL specification is 95% (V / V) ethanol and 4g composite catalyst {2g gac, 1g Fe(OH) 3 , 1g Al(OH) 3} into the four-necked flask, stirred for 0.5 hours, and began to heat. When the temperature rose to 65°C, 45.8g of hydrazine hydrate (80%) was slowly dripped into the four-necked flask from the constant pressure funnel, and the dropping time was 1 ~3 hours, continue to react at 60~80°C for 2~6 hours after dropping, stop the reaction, cool down to 30°C, and obtain the filtrate by suction filtration, which is 2,4-dichloro-5-isopropoxyaniline solution . The weight of the filtrate was 259.8 g, the content of 2,4-dichloro-5-isopropoxyaniline in the filtrate was 28.3%, and the reaction yield was 91.2%. ...

Embodiment 3

[0029] With 2,4-dichlorophenol as the starting material, 100g of 2,4-dichloro-5-isopropoxynitrobenzene (content 91.6% ) into the four-necked bottle, which is respectively equipped with a thermometer, an electric stirring device, a condenser and a constant pressure funnel, and the 150mL specification is 95% (V / V) ethanol and 60g composite catalyst {30g gac, 15g Fe(OH) 3 , 15g Al(OH) 3} into the four-necked flask, stirred for 0.5 hours, and began to heat. When the temperature rose to 65°C, 45.8g of hydrazine hydrate (80%) was slowly dripped into the four-necked flask from the constant pressure funnel, and the dropping time was 1 ~3 hours, continue to react at 60~80°C for 2~6 hours after dropping, stop the reaction, cool down to 30°C, and obtain the filtrate by suction filtration, which is 2,4-dichloro-5-isopropoxyaniline solution . The weight of the filtrate was 249.8 g, the content of 2,4-dichloro-5-isopropoxyaniline in the filtrate was 30.8%, and the reaction yield was 95.4...

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Abstract

The invention relates to a synthesis method of 2,4-dichloro-5-isopropoxy aniline. The method is characterized in that 2,4-dichloro-5-isopropoxy nitrobenzene with an empirical formula of C9H9NO3Cl2 is used as a raw material, and alcohol is used as a solvent; and in the presence of the action of a composite catalyst, hydrazine hydrate with a molecular formula of N2H4.H2O is added by adopting a dropping mode to synthesize the 2,4-dichloro-5-isopropoxy aniline the empirical formula of which is C9H11NOCl2. The invention not only can obviously improve the yield of the reaction and the product quality and greatly reduce the generation quantity of waste dreg and waste water, but also can simplify the post operation difficulty and shorten the post operation time.

Description

technical field [0001] The invention relates to a method for synthesizing an intermediate of the herbicide oxadiazone, specifically a method for synthesizing 2,4-dichloro-5-isopropoxyaniline. technical background [0002] 2,4-dichloro-5-isopropoxyaniline is an important intermediate for the synthesis of herbicide oxadiazon, which is generally produced by reduction reaction of 2,4-dichloro-5-isopropoxynitrobenzene be made of. There are many ways to realize this process, but the method that has been widely used for a long time is the iron powder reduction method. The iron powder reduction method has the advantages of good selectivity and low synthesis cost, but this method also has a large amount of "three wastes". The process operation is cumbersome, the synthetic yield is low, and the shortcomings such as poor product quality. Iron powder reduction method synthesizes 2, the reaction formula of 4-dichloro-5-isopropoxyaniline is as follows: [0003] Contents of the inve...

Claims

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Application Information

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IPC IPC(8): C07C217/84C07C213/02
Inventor 韩谋国王多余高巍
Owner ANHUI KELIHUA CHEM
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