Method for preparing pentachlorobenzoyl chloride

A technology of pentachlorobenzoyl chloride and polychlorobenzoyl chloride, which is applied in the field of preparation of pentachlorobenzoyl chloride, can solve the problems of difficult preparation, incomplete reaction, and high equipment requirements, and achieves less three wastes, simple and safe operation, and high process efficiency. reasonable effect

Active Publication Date: 2009-04-29
SHANGHAI HETENG FINE CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Patent DE2931688 discloses to generate pentachlorobenzoic acid with the reaction of pentachlorotrifluoromethylbenzene and concentrated sulfuric acid, then refluxes with thionyl chloride to generate pentachlorobenzoyl chloride (reaction formula is as follows), the disadvantage of this method is that raw material five Chlorotrifluoromethylbenzene is as difficult to prepare as the product pentachlorobenzoyl chloride
The lack of reaction is that the reaction is not complete, and the requirements for equipment are relatively high under high pressure, high temperature and high corrosion reaction.

Method used

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  • Method for preparing pentachlorobenzoyl chloride
  • Method for preparing pentachlorobenzoyl chloride
  • Method for preparing pentachlorobenzoyl chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Add 1200 milliliters (1460 grams) of benzoyl chloride, 1500 milliliters of chlorosulfonic acid, 1500 milliliters of carbon tetrachloride, 500 milliliters of thionyl chloride and 6 grams of iodine into the reaction flask, cool with ice water, and pass chlorine gas at 10 to 20 degrees to Reaction exothermic slows down, temperature is raised to 45~50 degrees slowly and keeps logical chlorine gas, GC is tracked to stop logical chlorine gas when the conversion ratio of pentachlorobenzoyl chloride to benzoyl chloride or polychlorobenzoyl chloride reaches 98%, and then After reacting at 55-60°C for one hour, keep the temperature below 10°C and pour the reaction mixture into a mixture of ice and carbon tetrachloride, then extract, separate layers, and concentrate the carbon tetrachloride layer to obtain the finished pentachlorobenzyl Acid chloride 3052 g, yield: 93.9%.

Embodiment 2

[0030] Add 200 milliliters (243 grams) of benzoyl chloride, 500 milliliters of chlorosulfonic acid, 500 milliliters of carbon tetrachloride, 10 milliliters of thionyl chloride and 1 gram of iodine into the reaction flask, cool with ice water at 10-20 degrees, and pass chlorine gas to react Exothermic slowing down, temperature is raised to 50~55 degrees slowly and keeps logical chlorine gas, GC is tracked to stop logical chlorine gas when the conversion ratio of pentachlorobenzoyl chloride to benzoyl chloride or polychlorobenzoyl chloride reaches 98%, and then After reacting at 50-55°C for one hour, distill the reaction mixture to an internal temperature of 90°C to recover carbon tetrachloride and thionyl chloride, and then distill under reduced pressure (25mmHg) to recover chlorosulfonic acid to obtain the finished pentachlorobenzyl Acid chloride 520 g, yield: 96%.

[0031] The recovered solvent can be directly used in the preparation of the next batch of pentachlorobenzoyl ch...

Embodiment 3

[0033] Add 200 milliliters (299 grams) of 2,4-dichlorobenzoyl chloride, 300 milliliters of chlorosulfonic acid, 350 milliliters of thionyl chloride and 1 gram of iodine into the reaction flask, cool with ice water at 30-35 degrees, and pass chlorine gas until the reaction releases. Heat slows down, and temperature is raised to 50~55 degrees slowly and keeps logical chlorine gas, and GC tracks to stop logical chlorine gas when the conversion rate of pentachlorobenzoyl chloride to benzoyl chloride or polychlorobenzoyl chloride reaches 98%, and then at 50 ~55 degrees of reaction for one hour, the reaction mixture was first atmospherically distilled to an internal temperature of 90 degrees to reclaim thionyl chloride, and then reduced pressure (25mmHg) to distill and reclaim chlorosulfonic acid to obtain 421 grams of finished product pentachlorobenzoyl chloride. : 94.3%.

[0034] The recovered solvent can be directly used in the preparation of the next batch of pentachlorobenzoyl ...

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PUM

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Abstract

The invention relates to a preparation method of pentachlorobenzoyl chloride, which is characterized in that, benzoyl chloride or polychlorobenzoyl chloride is used as the raw material; chlorosulfuric acid, carbon tetrachloride and thionyl chloride, or chlorosulfuric acid, carbon tetrachloride and sulfuryl chloride are used as the mixed solvent; iodine is the catalyst, and chlorine is the chlorination agent. Compared with prior art, the preparation method has the advantages of reasonable process, simple and safe operation, a high productivity as much as 96 percent, recyclable solvent, less three wastes, environmental protection and energy saving, and adaptability for industrial production.

Description

technical field [0001] The invention relates to pesticides and pharmaceutical intermediates, in particular to a preparation method of pentachlorobenzoyl chloride. Background technique [0002] As an important pesticide and pharmaceutical intermediate, pentachlorobenzoyl chloride has been partially reported in foreign open technologies. [0003] Document Mem.Fac.Sci., 16 (1), 47-50 (1987) has reported that take hexachlorobenzene as raw material, BuLi as catalyzer, reacts with carbon dioxide to generate pentachlorobenzoic acid (reaction formula is as follows), pentachlorobenzoic acid Thionyl chloride can be refluxed to generate pentachlorobenzoyl chloride. This method is only suitable for laboratory preparation and is difficult to industrialize. [0004] [0005] Patent DE2931688 discloses to generate pentachlorobenzoic acid with the reaction of pentachlorotrifluoromethylbenzene and concentrated sulfuric acid, then refluxes with thionyl chloride to generate pentachlorobenz...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C63/70C07C51/363
Inventor 施冠成滑国钰
Owner SHANGHAI HETENG FINE CHEM
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