Preparation method for aryl sulfonyl chloride derivative

A technology of arenesulfonyl chloride derivatives and products, which is applied in the field of preparation of arenesulfonyl chloride derivatives, can solve problems such as easy production of by-products, easy production of sulfur, and large amount of chlorosulfonic acid, so as to avoid pollution and ensure Purity, the effect of reducing production costs

Inactive Publication Date: 2015-12-02
TAIXING ZHENQING CHEM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The invention discloses a preparation method of arenesulfonyl chloride derivatives, which is used to solve the problems of easy generation of by-products,

Method used

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  • Preparation method for aryl sulfonyl chloride derivative
  • Preparation method for aryl sulfonyl chloride derivative
  • Preparation method for aryl sulfonyl chloride derivative

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[0029] A preparation method of arene sulfonyl chloride derivatives, comprising the following steps:

[0030] 1) Preparation of chlorosulfonic acid: add a certain amount of hydrogen chloride gas and sulfur trioxide gas into the synthesizer, control the temperature at 115-130°C, cool after a period of reaction, and then separate to obtain chlorosulfonic acid for use;

[0031] 2) Preparation of crude aromatic alkyl sulfonyl chloride derivatives: add 2 to 6 moles of chlorosulfonic acid into the three-necked flask, and simultaneously feed 0.5 to 1.5 moles of sulfur trioxide gas to form a stable chlorosulfonic acid solution, and then pour the three-necked flask Slowly add 1 mole of aromatic hydrocarbon-based derivatives, and drop 1-2 drops of acetic acid at the same time, raise the temperature to 50-140 ° C, keep the temperature constant, react for 6-8 hours, and then lower the temperature in the three-necked flask to 40-60°C, add 0.5-3 moles of phosphorus oxychloride dropwise, then...

Embodiment 1

[0035] Add 233.04g of chlorosulfonic acid into a three-necked flask equipped with a thermometer and a stirrer, and introduce 40.03g of sulfur trioxide gas to form a stable chlorosulfonic acid solution, then slowly add 123.11g of nitrobenzene, and dropwise add 1 to 2 Drop acetic acid, raise the temperature to 50°C, stir and react at this temperature for 6h, after the end of the reaction, lower the temperature to 40°C, continue to drop 76.67g of phosphorus oxychloride into the three-necked flask, and raise the temperature to 60°C °C, react at this temperature for 2 hours, after the reaction is complete, lower the temperature to below 20 °C, and at the same time pass the hydrogen chloride gas generated by the reaction into water, the hydrogen chloride gas will be dissolved in water to generate hydrochloric acid as a by-product, and the crude aromatic hydrocarbon Acid chloride derivatives were added to ice water, stirred and diluted, and 1231.1g of carbon tetrachloride was added fo...

Embodiment 2

[0037] Add 699.12g of chlorosulfonic acid into a three-necked flask equipped with a thermometer and a stirrer, and introduce 120.09g of sulfur trioxide gas to form a stable chlorosulfonic acid solution, then slowly add 123.11g of nitrobenzene, and dropwise add 1 to 2 Drop acetic acid, raise the temperature to 50°C, stir and react at this temperature for 6h, after the end of the reaction, lower the temperature to 40°C, continue to drop 459.99g of phosphorus oxychloride into the three-necked flask, and raise the temperature to 60°C °C, react at this temperature for 2 hours, after the reaction is complete, lower the temperature to below 20 °C, and at the same time pass the hydrogen chloride gas generated by the reaction into water, the hydrogen chloride gas will be dissolved in water to generate hydrochloric acid as a by-product, and the crude aromatic hydrocarbon Acid chloride derivatives were added to ice water, stirred and diluted, and 1477.32g of carbon tetrachloride was added...

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Abstract

The invention discloses a preparation method for an aryl sulfonyl chloride derivative. The aryl sulfonyl chloride derivative is prepared through the following steps that firstly, an aryl derivative is slowly added in a mixture of chlorosulfonic acid and sulfur trioxide, 1-2 drops of acetic acid is dropwise added, the temperature is increased to 50-140 DEG C and is kept invariable, and a reaction is performed for 6-8 h; secondly, the temperature is lowered to 40-60 DEG C, phosphorus oxychloride is dropwise added, then the temperature is increased to 60-120 DEG C, and a heat preservation reaction is performed for 2-4 h; thirdly, after the complete reaction is achieved, the temperature is lowered below 20 DEG C, and the mixture is added into ice water for dilution; finally, solvent is added, and the aryl sulfonyl chloride derivative is prepared after distillation and filtration are performed. According to the preparation method, the reaction is stable, the demand quantity for the chlorosulfonic acid is little, the product yield is high, and the problem that in a normal reaction, sulphur is generated due to the fact that a disproportionated reaction takes place between the added phosphorus trichloride and sulfuric acid is solved; meanwhile, no hydrogen chloride gas is generated, aftertreatment is convenient, and pollution to the environment is little.

Description

technical field [0001] The invention relates to the technical field of dyestuff chemical intermediate manufacture, in particular to a preparation method of arenesulfonyl chloride derivatives. Background technique [0002] Arylalkylsulfonyl chloride derivatives can be prepared by reacting arene derivatives with excess chlorosulfonic acid, because —SO 2 The Cl group is very active and can be easily converted into a sulfonamide (—SO 2 NH 2 ), substituted sulfonamides (—SO 2 NHR), reduced to thiophenol (—SH) and reductively condensed to m-(β-hydroxyethyl sulfone) aniline, which becomes an intermediate for the synthesis of drugs or dyes. It has a wide range of uses and is very important in the synthesis of fine chemicals. significance. At present, most of the aromatic hydrocarbon derivatives are chlorosulfonated with excess chlorosulfonic acid in the market, and then the reactant is diluted with a large amount of ice cubes, and used after precipitation and filtration. The rea...

Claims

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Application Information

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IPC IPC(8): C07C309/86C07C303/02C07C303/08
Inventor 杨继群张业容姚勇
Owner TAIXING ZHENQING CHEM CO LTD
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