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Synthesis method of 3,5-dichlorobenzoyl chloride

A technology of dichlorobenzoyl chloride and a synthesis method is applied in the synthesis field of 3,5-dichlorobenzoyl chloride, and can solve the problems of large amount of hazardous chemicals, low production safety, three wastes and corrosion, etc. The effect of high safety, high product yield and high industrial value

Active Publication Date: 2018-05-25
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

[0010] 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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  • Synthesis method of 3,5-dichlorobenzoyl chloride

Examples

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Comparison scheme
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Embodiment 1

[0017] Example 1 Synthesis of 3,5-dichlorobenzoyl chloride

[0018] Add 265.5 grams (1.0 moles) of trimesoyl chloride and 2.7 grams of Ni-Co / Al to a 500 mL four-necked bottle 2 o 3 Catalyst, heated to 180°C with stirring, kept the temperature for 32 hours, distilled under reduced pressure, collected 125-128°C fraction (1.73kPa) to obtain 187.7g of 3,5-dichlorobenzoyl chloride, yield 89.6%, content 98.37%.

Embodiment 2

[0019] Example 2 Synthesis of 3,5-dichlorobenzoyl chloride

[0020] Add 228.3 grams (0.86 moles) of trimesoyl chloride and 6.8 grams of Ni / Al to a 500 mL four-necked bottle 2 o 3 Catalyst, heat up to 220°C with stirring, keep the temperature for 18 hours, distill under reduced pressure, collect 125-128°C fraction (1.73kPa) to obtain 164.5g of 3,5-dichlorobenzoyl chloride, yield 91.3%, content 98.13%.

Embodiment 3

[0021] Example 3 Synthesis of 3,5-dichlorobenzoyl chloride

[0022] Add 318.6 grams (1.2 moles) of trimesoyl chloride and 10.5 grams of Ni-Cu / Al to a 500 mL four-necked bottle 2 o 3 Catalyst, heat up to 200°C with stirring, keep warm for 22 hours, distill under reduced pressure, collect 125-128°C fraction (1.73kPa) to obtain 233.8g of 3,5-dichlorobenzoyl chloride, yield 93.0%, content 98.27%.

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Abstract

The invention discloses a synthesis method of 3,5-dichlorobenzoyl chloride. The method is characterized in that trimesoyl chloride is taken as a raw material, and two carbon monoxides are directly removed under the action of nickel or a nickel-based catalyst, and thus the 3,5-dichlorobenzoyl chloride is obtained. Compared with the conventional preparation method, the synthesis method of the 3,5-dichlorobenzoyl chloride, disclosed by the invention, has the characteristics of short reaction flow, low catalyst price, few three wastes, no need of recovering and treating a large amount of dangerousby-products, lower production cost and the like; the synthesis method of the 3,5-dichlorobenzoyl chloride is suitable for industrial production.

Description

technical field [0001] The invention relates to a synthesis method of 3,5-dichlorobenzoyl chloride, which belongs to the field of fine organic chemical industry. Background technique [0002] 3,5-Dichlorobenzoyl chloride is an important intermediate in organic synthesis, widely used as an intermediate in medicines and pesticides, such as in the synthesis of the herbicide pentoxychlor. [0003] The synthetic routes of 3,5-dichlorobenzoyl chloride mainly contain the following: [0004] 1. U.S. Patent US 3931300, Chemical Industry Progress (2002, 21 (10), 756-757), German Patent DE 2659147, etc. reported that anthranilic acid, p-aminobenzoic acid or a mixture of the two were 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 the amino group is eliminated by diazotization reduction to obtain 3,5-dichlorobenzoic acid, and finally chlorinated by the chlorinating agent chlorine 3,5-dichl...

Claims

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Application Information

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IPC IPC(8): C07C51/62C07C63/70
CPCC07C51/62C07C63/70
Inventor 吴美宁王农跃茅晓晖郑建霖程小霞聂孝文郑土才
Owner 江西吉翔医药化工有限公司
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