Method for synthesizing 3,5-dichlorobenzoyl chloride

A technology for the synthesis of dichlorobenzoyl chloride and its synthesis method, which is applied in the field of synthesis of 3,5-dichlorobenzoyl chloride, an intermediate of agricultural chemicals, and can solve the problems of large amount of hazardous chemicals, low production safety, three wastes and corrosion and other issues, to achieve the effects of high production safety, high product yield, and mild reaction conditions

Active Publication Date: 2014-01-15
江西吉翔医药化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0022] In order to overcome the shortcomings of the existing 3,5-dichlorobenzoyl chloride preparation technology, such as three wastes, serious corrosion, large amount of hazardous chemicals, low production safety, high cost, and low product content, the present invention provides a 3,5-dichlorobenzoyl chloride preparation technology. The synthetic method of 5-dichlorobenzoyl chloride

Method used

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  • Method for synthesizing 3,5-dichlorobenzoyl chloride
  • Method for synthesizing 3,5-dichlorobenzoyl chloride
  • Method for synthesizing 3,5-dichlorobenzoyl chloride

Examples

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Embodiment 1

[0033] Example 1 Heat 140.5g (1.0mol) of benzoyl chloride to 130°C, add 176g (2.2mol) of sulfur trioxide dropwise, and control the dropping for 2 hours. During the dropwise addition, the temperature was gradually raised to 170°C, and continued to be raised to 220°C after the dropwise addition and kept for 16 hours. After cooling to 120°C, 2.0 g of catalyst 4-dimethylaminopyridine (DMAP) and 60 g of mixed xylene were added. Within 1 hour, 218 g (2.2 mol) of triphosgene was added in 6 batches, and the reaction was kept for 3 hours. The solvent was recovered by distillation under reduced pressure until the inner temperature reached 150°C. At a temperature of 175° C., chlorine gas is passed into the reaction solution under the liquid surface at a rate of 0.4 g / min, and sulfur dioxide gas escapes immediately. After 2.5 hours of reaction, no more sulfur dioxide was released. Cool to 50°C and distill under reduced pressure to obtain 182g of crude product with a yield of 86.8%, ...

Embodiment 2

[0034] Example 2 Heat 140.5g (1.0mol) of benzoyl chloride to 140°C, add 176g (2.2mol) of sulfur trioxide dropwise, and control the dropping for 2 hours. During the dropwise addition, the temperature was gradually raised to 170°C, and continued to be raised to 220°C after the dropwise addition and kept for 16 hours. After cooling to 100° C., 1.1 g of a catalyst triethylenediamine (DABCO) and 50 g of chlorobenzene were added. Within 1 hour, 218 g (2.2 mol) of triphosgene was added in 6 batches, and the reaction was kept for 4 hours. The solvent was recovered by distillation under reduced pressure until the inner temperature reached 150°C. Under the condition of heat preservation, chlorine gas is fed under the liquid surface of the reaction solution at a rate of 0.4 g / min, and sulfur dioxide gas escapes immediately. After 2.0 hours of reaction, no sulfur dioxide is released. Cooled to 50°C and distilled under reduced pressure to obtain 179g of crude product with a yield of...

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Abstract

The invention discloses a method for synthesizing 3,5-dichlorobenzoyl chloride. The method comprises the following steps: carrying out sulfonation on benzoyl chloride by sulfur trioxide to obtain 5-chloroformyl metaphenylene disulfonic acid; carrying out chlorination by catalyzed triphosgene to obtain 5-chloroformyl metaphenylene disulfuryl chloride; finally, carrying out removal of sulfur dioxide chlorination to obtain 3,5-dichlorobenzoyl chloride. Compared with an existing preparation method, the method disclosed by the invention has the characteristics of stable chlorinating agent, high production safety, small amount of three wastes, no requirement for recovering and treating a great amount of dangerous byproducts, no requirement for refining a coarse product, low production cost and the like and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of fine chemicals, in particular to a method for synthesizing an agricultural chemical intermediate 3,5-dichlorobenzoyl chloride. Background technique [0002] 3,5-Dichlorobenzoyl chloride is a widely used fine chemical intermediate, especially an important intermediate for the synthesis of herbicides propyzamide, oxaziclomefone and tridiphane . [0003] [0004] [0005] The literature synthesis routes of reported 3,5-dichlorobenzoyl chloride mainly contain the following: [0006] 1. American patent US 3931300, chemical engineer (2009, (6), 68-70), chemical industry progress (2002, 21 (10), 756-757), German patent DE 2721133, German patent DE 2659147, etc. reported o-aminobenzene Formic acid, p-aminobenzoic acid or a mixture of the two are chlorinated by a chlorinating agent to obtain 3,5-dichloroanthranilic acid, 3,5-dichloro-p-aminobenzoic acid or a mixture of the two, and then diazotized Reductive eliminati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C63/70C07C51/62
CPCC07C51/62C07C303/02C07C303/06C07C63/70C07C309/58C07C309/89
Inventor 郑土才聂孝文况庆雷郑建霖魏源陈锋王吉
Owner 江西吉翔医药化工有限公司
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