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Method for synthesizing 2,4-Dichlorobenzoyl chloride

A technology of dichlorobenzoyl chloride and dichlorotrichlorotoluene, which is applied in the field of intermediate synthesis of compounds, can solve the problems of harsh working environment, unstable product quality, and not pleasant enough, and achieve high space-time yield

Inactive Publication Date: 2007-09-19
江苏强盛功能化学股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Both have certain practicability, such as the former has a simple process; the latter has a high yield and is simple to purify; but both have corresponding defects, such as the former has unstable product quality; the latter produces a part of hydrogen chloride simultaneously. Partial sulfur dioxide brings certain difficulties to tail gas treatment, and the working environment is harsh and not pleasant enough

Method used

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  • Method for synthesizing 2,4-Dichlorobenzoyl chloride

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Embodiment 1

[0021] Add raw material 2,4-dichlorobenzoic acid 529g (2.0mol), 2,4-dichlorobenzoic acid 382 (2mol), toluene 500ml, catalyst aluminum trichloride 0.13g (0.001mol) into the reactor, adjust The temperature was raised to 120°C, and the reaction was kept for 240 minutes. Sampling analysis: the yield of 2,4-dichlorobenzoyl chloride was 98.8%. Then distill and reclaim toluene, and then collect the finished product of 2,4-dichlorobenzoyl chloride by distillation under reduced pressure; the catalyst aluminum trichloride is recovered from the still residue for the next feeding.

[0022] Result: bp.122-124°C / 15mm, 2,4-dichlorobenzoyl chloride, colorless to pale yellow liquid, GC content 99.22%.

Embodiment 2

[0024] Add 529g (2.0mol) of raw material 2,4-dichlorobenzotrichloride and 0.98g (0.01mol) of catalyst phosphoric acid into the reactor, adjust the temperature to 60°C, add 108g (1.80mol) of acetic acid dropwise, and maintain the temperature of the reactor The temperature was 60°C, and the dropwise addition was completed in about 120 minutes. After the dropwise addition of acetic acid, the insulation reaction was continued for 60 min and the previous fraction was collected. 2,4-Dichlorotrichlorotoluene reacts rapidly with acetic acid under the action of catalyst phosphoric acid to generate acetyl chloride, which is separated from the reactor as the first fraction from the top of the rectifying tower.

[0025] Sampling analysis: the yield of 2,4-dichlorobenzoyl chloride was 90.3%. Then the finished product of 2,4-dichlorobenzoyl chloride was collected by distillation under reduced pressure, which was normal boiling.

[0026] result:

[0027] Front fraction: 50-55℃, acetyl chl...

Embodiment 3

[0030] Add 529g (2.0mol) of the raw material 2,4-dichlorobenzotrichloride and 1.62g (0.01mol) of the catalyst iron trichloride into the reactor, adjust the temperature to 120°C, add 151g (2.04mol) of propionic acid dropwise, and maintain The temperature of the reaction kettle is 120-130°C, and the dropwise addition is completed in about 120 minutes. 2,4-dichlorotrichlorotoluene and propionic acid react rapidly under the action of catalyst ferric chloride to generate propionyl chloride, which is separated from the reactor from the top of the rectifying tower as the first component. After the dropwise addition of propionic acid, the insulation reaction was continued for 210 min. Sampling analysis: the yield of o-chlorobenzoyl chloride is 98.6%. Then, the crude product of propionyl chloride is distilled under reduced pressure in the rectifying tower as the middle distillate, and the crude product of 2,4-dichlorobenzoyl chloride is in the still; the 2,4-dichlorobenzoyl chloride f...

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Abstract

A method for synthesizing the 2,4-dichlorobenzoyl chloride belongs to a field of intermediate synthesis of the compound, including catalyzing the 2,4-dichlorobenzotrichloride and carboxylic acid to produce single or compound coarse acyl chloride in the effect of the catalyzer; then rectifying to get corresponding acyl chloride. The advantages of the invention is that environment of the production is clean; the catalyzer can be recycled; carbonyl chloride with low boiling point may be drived off in time so as to get a high empty yield.

Description

technical field [0001] The invention relates to a method for synthesizing 2,4-dichlorobenzoyl chloride, which belongs to the technical field of compound intermediate synthesis. technical background [0002] 2,4-Dichlorobenzoyl chloride is an important intermediate in organic synthesis, widely used in the fields of pesticides, medicines and organic peroxides, and is an important acylation and benzylation reagent. At present, the methods for preparing 2,4-dichlorobenzoyl chloride mainly include: 2,4-dichlorobenzoyl chloride hydrolysis method and 2,4-dichlorobenzoic acid and thionyl chloride co-heating method. Both have certain practicability, such as the former has a simple process; the latter has a high yield and is simple to purify; but both have corresponding defects, such as the former has unstable product quality; the latter produces a part of hydrogen chloride simultaneously. Partial sulfur dioxide brings certain difficulties to tail gas treatment, and the working envir...

Claims

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Application Information

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IPC IPC(8): C07C63/70C07C63/04C07C51/58
Inventor 曲大伟应志耀陆靖
Owner 江苏强盛功能化学股份有限公司
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