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Method for preparing 3-chlorosulfonylbenzoyl chloride

A technology of chlorosulfonylbenzoyl chloride and benzoic acid, which is applied in the fields of sulfonic acid preparation, acyl halide preparation, organic chemistry, etc., and can solve problems such as difficult recovery of thionyl chloride, difficulty in meeting production needs, and high energy consumption required for separation , to achieve the effect of good product quality, sufficient resources, and reduced complexity

Inactive Publication Date: 2018-08-14
江苏佳麦化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] Although the above-mentioned various industrial production methods are simple to operate, they all have disadvantages in varying degrees.
Trichlorobenzyl reacts with chlorosulfonic acid, and the yield is high, but it is easy to produce 4-(sulfonyl)benzoyl chloride and 3,5-disulfonylbenzoyl chloride in the reaction process, and requires a higher energy consumption; trichlorobenzyl reacts with oleum, except that it is easy to generate by-products and cause high energy consumption required for separation, and the yield is also relatively low, only about 60%; benzoic acid and chlorosulfonic acid, thionyl chloride prepare product , the yield is high, but due to the reaction of excess thionyl chloride with the water produced by chlorosulfonation to generate sulfur dioxide and hydrogen chloride, it is difficult to recover thionyl chloride, so the reaction liquid needs to be post-treated before entering the distillation system, which increases the complexity of the operation As for several other industrial methods, although the operation is simple and the yield is not low, the required raw materials, such as dipotassium m-sulfonic acid benzoate, are uncommon raw materials in the market, and it is difficult to meet the production demand; as for m-carboxybenzene yellow acid and carbon tetrachloride to prepare 3-chlorosulfonylbenzoyl chloride, the reaction conditions are harsh, and the required equipment requirements are also very high

Method used

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  • Method for preparing 3-chlorosulfonylbenzoyl chloride
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  • Method for preparing 3-chlorosulfonylbenzoyl chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Put 500g of benzoic acid and 668g of chlorosulfonic acid into a reactor with a slight negative pressure alkali absorption device, start stirring, add 5g of oleum, the closed reactor starts to heat up, and starts to keep warm at 80°C, GC gas spectrum Instrument tracking, after 14h, the amount of benzoic acid ≤ 0.05%, the reaction ended. Lower the temperature of the system to 8°C, start adding water dropwise while stirring, and the temperature rises slightly at first. After the 28g water is added dropwise, the temperature will not change, and then 28g water can be added at one time (because the reaction between water and excess chlorosulfonic acid is more intense) , belongs to the exothermic process, so the amount of water added dropwise is based on the temperature no longer changing. At this time, record the amount of water added dropwise, and then continue to add the same amount of water), stir for a while, let stand, separate layers, and the lower layer About 850g of t...

Embodiment 2

[0035] Put 500g of benzoic acid and 763g of chlorosulfonic acid into a reactor with a slight negative pressure alkali absorption device, start stirring, add 7.5g of fuming sulfuric acid, the closed reactor starts to heat up, and starts to keep warm at 90°C, GC gas Spectrometer tracking, after 11 hours, the amount of benzoic acid ≤ 0.05%, the reaction is over. Lower the temperature of the system to 8°C, start to add water dropwise while stirring, at first the temperature rises slightly, after the 45g of water is added dropwise, the temperature will not change, then you can add 45g of water at a time, stir for a while, let it stand, and separate About 862g of the sulfonated liquid in the lower layer was transferred to another reactor, and 86g of anhydrous sodium sulfate was added to stir for 1 hour, and filtered to obtain 851g of the sulfonated liquid for use. The upper water layer is neutralized with alkaline water and then poured into the waste water tank.

[0036] Put 2553g ...

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Abstract

The invention discloses a method for preparing 3-chlorosulfonylbenzoyl chloride. The method comprises the following steps: (1) benzoic acid and excess chlorosulfonic acid are subjected to a sulfonylation reaction with 20 wt% fuming sulfuric acid as a catalyst to prepare a sulfonating liquid; and (2) the sulfonating liquid prepared in the step (1) and oxalyl chloride are subjected to an acylation reaction with DMF as a catalyst to prepare the target product 3-chlorosulfonylbenzoyl chloride. The method has mild reaction conditions, short reaction time, simple operation, high yield, good productquality, and almost no pollution to environment, is suitable for industrial production, and has a very good application prospect.

Description

technical field [0001] The invention relates to a method for synthesizing 3-chlorosulfonylbenzoyl chloride, which belongs to the technical field of fine chemical organic synthesis. Background technique [0002] 3-Chlorosulfonylbenzoyl chloride is an important organic synthesis intermediate, molecular formula: C 7 h 4 Cl 2 o 3 S, CAS: 4052-92-0, the structural formula is as follows: [0003] [0004] 3-Chlorosulfonylbenzoyl chloride is an important intermediate in the synthesis of pesticides, food additives, and drugs, especially 3-chlorosulfonylbenzoyl chloride is used as a cross-linking agent to synthesize poly-2-ethyleneimidazoline reverse osmosis composite membranes and is widely used in Sewage treatment, seawater desalination, and picric water increase the demand for 3-chlorosulfonylbenzoyl chloride. Therefore, the research on the synthesis of 3-chlorosulfonylbenzoyl chloride is a subject of great interest to practitioners . [0005] At present, the most commonl...

Claims

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Application Information

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IPC IPC(8): C07C303/08C07C303/22C07C309/89C07C51/04C07C55/06
CPCC07C51/04C07C303/08C07C303/22C07C309/89C07C55/06
Inventor 刘学峰徐松汪港郭维成
Owner 江苏佳麦化工有限公司
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