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A kind of synthetic method of 3-chloromethylbenzoyl chloride

A technology of chloromethylbenzoyl chloride and a synthetic method, applied in the synthesis of 3-chloromethylbenzoyl chloride and the field of preparation of organic intermediates, can solve the production environment and surrounding environmental hazards, reduce product purity and yield, Increase the difficulty of separation and purification to achieve the effects of improving production safety, improving purity and yield, and reducing inorganic metal ions

Active Publication Date: 2017-07-07
湖北相和精密化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But there are obvious defects and deficiencies in the above-mentioned method: the one, 3-methylbenzoic acid photochlorination substitution reaction easily produces 3-(dichloromethyl)benzoic acid and 3-(trichloromethyl)benzoic acid by-products, Reduce the purity and yield of the product, and increase the difficulty of subsequent separation and purification; secondly, the photochlorination substitution reaction of 3-methylbenzoic acid needs to use chlorine gas, and phosphorus pentachloride needs to be used in the acyl chloride reaction of 3-chloromethylbenzoic acid Chlorine gas, phosphorus pentachloride and their decomposition products are highly toxic. On the one hand, the requirements for the sealing of production equipment are increased, and investment is increased. On the other hand, it is easy to cause serious harm to the production environment and the surrounding environment.

Method used

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  • A kind of synthetic method of 3-chloromethylbenzoyl chloride
  • A kind of synthetic method of 3-chloromethylbenzoyl chloride
  • A kind of synthetic method of 3-chloromethylbenzoyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Put 100ml of dichloromethane into the autoclave, add 0.1mol of trichloromethylbenzene, 0.1mol of paraformaldehyde, 0.05mol of anhydrous aluminum trichloride, fill with nitrogen to 0.4Mpa, and react at 55℃~60℃ for 8h. Then cool down to room temperature, let off the nitrogen, take a sample and carry out GC (Gas Chromatography, gas chromatography) analysis, the area normalization method main peak area accounts for 90.4%, after comparing with the 3-chloromethylbenzoyl chloride reference substance, it is confirmed that The target product is 3-chloromethylbenzoyl chloride.

Embodiment 2

[0026] Put 130ml of chloroform into the autoclave, add 0.1mol of trichloromethylbenzene, 0.15mol of paraformaldehyde, 0.05mol of anhydrous zinc chloride, fill nitrogen to 0.2Mpa, react at 65°C to 70°C for 5h, then cool down to At room temperature, the nitrogen gas was vented, and samples were taken for GC analysis. The area of ​​the main peak accounted for 86.6% by the area normalization method. After comparison with the reference substance of 3-chloromethylbenzoyl chloride, it was confirmed that it was the target product 3-chloromethylbenzoyl chloride.

Embodiment 3

[0028] Put 80ml of carbon tetrachloride into the autoclave, add 0.1mol of trichloromethylbenzene, 0.12mol of paraformaldehyde, 0.02mol of anhydrous ferric chloride, fill with nitrogen to 0.1Mpa, and react at 20℃~25℃ for 20h , then cool down to room temperature, vent nitrogen, take samples for GC analysis, the area normalization method main peak area accounts for 84.3%, after comparing with 3-chloromethylbenzoyl chloride reference substance, it is confirmed that it is the target product 3-chloromethyl Benzoyl chloride.

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Abstract

The present invention relates to a 3-chloro methyl benzoyl chloride synthetic method, and the specific method is as follows: 3-chloro methyl benzoyl chloride is synthesized from benzenyl trichloride and paraformaldehyde in a solvent in aluminium trichloride, ferric chloride and other Lewis acid catalysts. The synthetic method is a one-step reaction, and is simple and easy to control, mild in reaction condition, and high in finished product yield, starting materials are cheap and readily available, production cost is low, the synthetic method is less in waste, the waste can be harmlessly processed, and the synthetic method is clean and environmentally-friendly.

Description

technical field [0001] The invention relates to a method for preparing an organic intermediate, in particular to a method for synthesizing 3-chloromethylbenzoyl chloride, which belongs to the technical field of chemical industry. Background technique [0002] As an important organic intermediate, 3-chloromethylbenzoyl chloride is widely used in chemical industry and pharmacy, and can be used to synthesize many products. At present, rarely have the synthetic method of document record 3-chloromethylbenzoyl chloride, the synthetic method usually adopted by those skilled in the art is to be starting raw material with 3-methylbenzoic acid, at first 3-methylbenzoic acid is passed through 3-Chloromethylbenzoic acid was prepared by photochlorination, and then 3-chloromethylbenzoyl chloride was obtained by acyl chloride. But there are obvious defects and deficiencies in the above-mentioned method: the one, 3-methylbenzoic acid photochlorination substitution reaction easily produces ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/58C07C63/70
CPCC07C51/58C07C63/70
Inventor 易章国殷少华董晓露
Owner 湖北相和精密化学有限公司
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