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Method for synthesizing 3-(beta-sulfate ethyl sulfuryl)-N-ethyl aniline

A technology of sulfate ethyl sulfone and synthesis method, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry and other directions, can solve the problems of difficulty in realizing industrialization, high production cost, difficult recycling and the like, and achieves the reduction of waste water. The effect of producing, reducing dosage and saving production cost

Inactive Publication Date: 2014-05-21
JIAXING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the organic solvent used in this method is water-soluble, and after the esterification is completed, it is difficult to recycle, making the production cost higher and difficult to realize industrialization

Method used

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  • Method for synthesizing 3-(beta-sulfate ethyl sulfuryl)-N-ethyl aniline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a 250mL three-necked flask with stirring and reflux separator, add 150mL toluene, 0.025mol dibenzyl dodecylamine, 0.05mol 3-(β-hydroxyethylsulfone)-N-ethylaniline and 0.1mol 98% sulfuric acid, stir and mix evenly, heat up to reflux for 8 hours, high performance liquid chromatography (HPLC) detects that the content of 3-(γ-hydroxyethylsulfone)-N-ethylaniline 3 Aqueous solution, fully stirred and reacted for 2h, allowed to stand for stratification, the upper layer solution was reserved for the next application, the lower layer was 3-(β-sulfate ethyl sulfone group)-N-ethylaniline aqueous solution, dried to obtain a solid product, obtained The HPLC purity of the product is >95%, the diazotization content is >80%, and the yield is >85%.

Embodiment 2

[0025] Add 0.05mol 3-(β-hydroxyethylsulfone)-N-ethylaniline and 0.075mol 80% sulfuric acid to the upper layer solution of Example 1 above, stir and mix evenly, heat up to reflux for 9h, and perform high performance liquid chromatography (HPLC) detection of 3-(β-hydroxyethyl sulfone group)-N-ethylaniline content3 Aqueous solution, fully stirred and reacted for 2-3 hours, standing for stratification, the upper layer solution is reserved for the next application, the lower layer is 3-(β-sulfate ethyl sulfone group)-N-ethylaniline aqueous solution, HPLC purity > 95% , diazotization content > 80%, yield > 90%.

Embodiment 3

[0027] Xylene was used to replace the toluene in Example 1, and other conditions were the same, the HPLC purity of the obtained product was >92%, and the yield was >85%.

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Abstract

The invention relates to a method for synthesizing 3-(beta-sulfate ethoxyl sulfuryl)-N-ethyl aniline. 3-(beta-ethoxyl sulfuryl)-N-ethyl aniline is used as a raw material and subjected to sulfuric acid esterification in a water-insoluble organic solvent by using 1 to 2 times esterifying agent in the presence of a tertiary amine. Compared with the traditional esterification synthetic method, the method has the advantages of low consumption of the esterifying agent, good product quality, high yield and little three wastes.

Description

technical field [0001] The invention relates to reactive dye intermediates in the field of fine chemicals. Background technique [0002] 3-(β-sulfate ethyl sulfone)-N-ethylaniline (I) is an important intermediate of reactive dyes, which is widely used in some special reactive dyes. 3-(β-sulfate ethylsulfone)-N-ethylaniline is generally prepared from 3-(β-hydroxyethylsulfone)-N-ethylaniline (II) through sulfate esterification. [0003] [0004] The traditional sulfuric acid esterification process is to use a large amount of excess concentrated sulfuric acid or fuming sulfuric acid to carry out esterification at room temperature. After the esterification is completed, the esterification reaction solution is diluted into ice water to precipitate the product. The esterification method is relatively simple. However, a large amount of low-concentration sulfuric acid wastewater will be produced during the production process, which will bring a great burden to environmental prot...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/36C07C315/04
Inventor 王专谢亚杰胡万鹏徐松
Owner JIAXING UNIV
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