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O-methoxy-beta-sulfuric ester ethyl sulfonyl aniline and preparation method thereof

A technology of ethyl sulfone aniline and oxygen pairs, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as complex production methods, high use cost, and effective content of only 95%, reaching The production method is simple and the effect of easy operation

Inactive Publication Date: 2009-12-16
韩朝忠 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the raw material o-methoxy p-β-sulfate ethyl sulfone aniline used in the synthesis of reactive blue 250 and other dyes, as far as we know, there is no domestic manufacturer producing it, and most of them rely on imports. It is not only expensive, but also costly to use High, and the effective content of the product is only up to 95%. At the same time, although we do not know much about its production method, according to the analysis, the production method is relatively complicated. what people expect

Method used

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  • O-methoxy-beta-sulfuric ester ethyl sulfonyl aniline and preparation method thereof
  • O-methoxy-beta-sulfuric ester ethyl sulfonyl aniline and preparation method thereof
  • O-methoxy-beta-sulfuric ester ethyl sulfonyl aniline and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0022] a. Acetylation

[0023] With 100 grams of anthranil, add in reaction kettle 1 99 grams of acetic anhydride solution with 1 hour and stir, temperature is controlled at 75 ℃-78 ℃, after adding, keep warm for 1 hour, use vacuum pump and condenser steam heating to evacuate, in The acetic acid generated by the reaction was evaporated under vacuum conditions, and the reactant was sliced ​​by a microtome to obtain 135 grams of o-methoxyacetanilide. The reaction formula is as follows:

[0024]

[0025] b. Sulfonation

[0026] Add 500 grams of chlorosulfonic acid and 50 grams of thionyl chloride into the reaction kettle II, start stirring, add 100 grams of the above-mentioned acetylated product o-methoxyacetanilide within 2 hours, and control the reaction temperature at 45°C-48°C. After the end point, slowly add the sulfonated solution into 3000 grams of ice water for dilution, the temperature is controlled at 10°C-15°C, after the dilution is completed, put the diluted solu...

Embodiment 2

[0038] a. Acetylation

[0039] Add 1000kg of anthranilic ether to 990kg of acetic anhydride solution in 2000L reactor I in 4 hours, start stirring, and control the temperature at 75°C-80°C. Vacuum, the acetic acid generated by the reaction was evaporated under vacuum conditions, and the reactant was sliced ​​by a slicer to obtain 1350 kg of acetylated product o-methoxyacetanilide.

[0040] b. Sulfonation

[0041] Add 5500kg of chlorosulfonic acid and 500kg of thionyl chloride into the 5000L reactor II, start stirring, add the above-mentioned o-methoxyacetanilide 1000kg within 10 hours, and control the reaction temperature at 45°C-48°C. After the end of the reaction, the The sulfonated solution is slowly added into a dilution pot containing 15000kg of ice water for dilution. The temperature is controlled at 10°C-15°C. Oxy-p-β-sulfonyl chloride acetanilide.

[0042] c. Restore

[0043] Add 1000kg of sodium bisulfite into the reaction kettle III containing 3000kg of water to ...

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Abstract

The invention discloses o-methoxy-beta-sulfuric ester ethyl sulfonyl aniline and a preparation method thereof. The o-methoxy-beta-sulfuric ester ethyl sulfonyl aniline is used as a raw material for synthesizing dyes such as reactive blue 250, and the like, and is prepared according to the following steps: o-aminoanisole is acetylized by using acetic anhydride solution; the obtained acetylized compound is sulfonated by using chlorosulfuric acid and thionyl chloride; the obtained sulfonate is reduced by using sodium bisulfite and sodium hydroxide; the reducing substances are condensed by using ethylene oxide; and the obtained condensation compound is esterified by using sulphuric acid to obtain the product. The reactions are realized by mixing, dissolution and stirring in a reaction container and adopting the methods of vacuum heating, slicing, diluting, clarification, washing, suction filtering, drying and crushing. The invention solves the problems that the prior product depends on import and has high use cost and complex process, and has the advantages of simple manufacture method, easy operation and high effective content up to more than 97 percent.

Description

technical field [0001] The invention relates to a kind of o-methoxy p-beta-sulfate ethyl sulfone aniline and a preparation method thereof, which are used as raw materials for synthesizing reactive blue 250 and other dyes. Background technique [0002] At present, the raw material o-methoxy p-β-sulfate ethyl sulfone aniline used in the synthesis of reactive blue 250 and other dyes, as far as we know, there is no domestic manufacturer producing it, and most of them rely on imports. It is not only expensive, but also costly to use high, and the effective content of the product is only 95%. At the same time, although we do not know much about its production method, the production method is relatively complicated according to analysis. what people expect. Contents of the invention [0003] The purpose of the present invention is exactly to provide a kind of o-methoxy p-beta-sulfate ethyl sulfone aniline and preparation method thereof for people, and it can overcome some defici...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/36C07C315/04
Inventor 韩朝忠段明发
Owner 韩朝忠
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