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Preparation method of para-ester

A para-ester and acetanilide technology, which is applied in the field of preparation of para-ester, can solve the problems of low chlorosulfonation yield and heavy pollution, and achieve the effects of high yield, increased yield and mild conditions

Inactive Publication Date: 2018-01-09
新乡市锦源化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a preparation method of para-ester, which solves the problems of low chlorosulfonation yield and large pollution when preparing para-ester

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Synthetic para-ester

[0045] Step 1: Synthesis of Acetanilide

[0046] Add 0.3 mol of aniline, 0.3 mol of ammonium chloride, 0.2 mol of glacial acetic acid, 0.4 mol of N,N-dimethylacetamide and 0.24 mol of dicyclohexylcarbodiimide into a round-bottomed flask, install an air condenser, Stir and heat up to 120°C, and reflux for 3 hours. After the reaction is complete, stop heating and cool to room temperature naturally.

[0047] Add ice water to the above reaction solution, let it stand, and when no solid precipitates out, filter it with suction, continue cooling the filtrate to below 0°C, and filter it with suction again, combine the solids obtained from the two suction filtrations, and wash with water , dried to obtain white needle crystals with a yield of 98.3%.

[0048] Step 2: Chlorosulfonation

[0049] First, add the measured mixture of 1.5mol chlorosulfonic acid and 1.2mol thionyl chloride into the reaction tank, then add about 1 mol of acetanilide into the sul...

Embodiment 2

[0057] The difference from Example 1 is mainly that the consumption of phosphorus pentoxide is different, specifically as follows.

[0058] Step 1: Chlorosulfonation

[0059] First, add the measured 1.5mol chlorosulfonic acid and 1.2mol thionyl chloride mixture into the reaction tank, then add about 1 mol of acetanilide (commercially available) into the sulfonation reaction tank at one time, and then add to the sulfonation Add 0.8mol phosphorus pentoxide into the reactor, then turn on the switch of the reactor, let the mixture of chlorosulfonic acid and thionyl chloride drip into the sulfonation reactor at the speed of 0.1mL / s, and control the reaction tank The temperature is 15°C. After the dropwise addition, let it stand for half an hour, the hydrogen chloride, SO 2 The gas is treated by two-stage liquid alkali absorption. After fully reacting, put frozen brine in the jacket to cool down, so that 4-acetamidobenzenesulfonyl chloride is precipitated, then filter and separate...

Embodiment 3

[0067] The difference with embodiment 1 mainly lies in the consumption difference of chlorosulfonic acid, specifically as follows.

[0068] Step 1: Chlorosulfonation

[0069] First, add the measured mixture of 2.5mol chlorosulfonic acid and 1.2mol thionyl chloride into the reaction tank, then add about 1 mol of acetanilide (commercially available) into the sulfonation reaction tank at one time, and then add it to the sulfonation reaction tank. Add 0.8mol phosphorus pentoxide into the reactor, then turn on the switch of the reactor, let the mixture of chlorosulfonic acid and thionyl chloride drip into the sulfonation reactor at the speed of 0.1mL / s, and control the reaction tank The temperature is 15°C. After the dropwise addition, let it stand for half an hour, the hydrogen chloride, SO 2 The gas is treated by two-stage liquid alkali absorption. After fully reacting, put frozen brine in the jacket to cool down, so that 4-acetamidobenzenesulfonyl chloride is precipitated, the...

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PUM

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Abstract

The invention provides a preparation method of para-ester. The preparation method of para-ester comprises the following steps: under the existence of phosphorus pentoxide, carrying out chlorosulfonation on N-phenylacetamide and chlorosulfonic acid as well as thionyl chloride, thus obtaining a chlorosulfonation composition; and sequentially carrying out reduction reaction, condensation reaction andesterification reaction on the chlorosulfonation composition, thus obtaining para-ester. Compared with the prior art, the preparation method has the advantages that phosphorus pentoxide is added in chlorosulfonation, a balance state is broken, the balance moves to the direction in which 4-acetamidobenzenesulfonyl azide is generated, the conversion rate of N-phenylacetamide is increased, namely the yield of chlorosulfonation is increased, and meanwhile, excessive chlorosulfonic acid is avoided, so that wastewater pollution is alleviated.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of para-ester. Background technique [0002] Para-ester, alias p-(β-sulfate ethyl sulfone) aniline, vinyl sulfone sulfate, 4-sulfate ethyl sulfone aniline, p-β-hydroxyethylsulfone aniline sulfate, p-β-hydroxyethylsulfone aniline Sulfate. Para-ester is an important intermediate of reactive dyes, and is used to synthesize reactive dyes containing vinylsulfone groups such as EF type, KN type, M / KM type, and ME type. [0003] The para-ester is a temporary water-soluble group, which can not only improve the solubility of the dye when it is applied, but also the reactive dye containing hydroxyethyl sulfone sulfate group has a low affinity to the fiber during dyeing, which may achieve the effect of level dyeing and generate Dye-fiber ether bond, ether bond has good acid resistance and thermal stability, which is beneficial to improve washing efficiency and wet fas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/04C07C317/36
Inventor 蔡红新樊明伟闫玲玲王书擘王元
Owner 新乡市锦源化工有限公司
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