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Preparation method of 3,5-dichlorobenzoyl chloride

A technology of dichlorobenzoyl chloride and benzoic acid, which is applied in the preparation of carboxylic acid amides, organic compounds, carboxylate, etc., can solve the problem of low yield and achieve the effect of preventing oxidation

Inactive Publication Date: 2016-08-31
SHANDONG RUNBO BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to, overcome the low yield problem of existing preparation 3,5-dichlorobenzoyl chloride method, provide a kind of novel preparation method of 3,5-dichlorobenzoyl chloride; The present invention provides The method for preparing 3,5-dichlorobenzoyl chloride effectively prevents the oxidation of the amino group, and the total yield is high

Method used

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  • Preparation method of 3,5-dichlorobenzoyl chloride
  • Preparation method of 3,5-dichlorobenzoyl chloride
  • Preparation method of 3,5-dichlorobenzoyl chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0047] Add 137g of anthranilic acid and 110g of acetic anhydride to a 1000mL four-necked flask, and perform the first reaction at 100°C. Stop the reaction when the impurity peak of the liquid chromatography reaches below 3% (the same below), and obtain 2-acetamidobenzene Formic acid (the required reaction time is about 12h). After the first reaction is over, add 500g of glacial acetic acid to the above-mentioned four-necked bottle, stir evenly, and then slowly introduce 150g of chlorine gas at 40°C to carry out the second reaction. Stop the reaction (the same below); the required reaction time is about 12 hours. After the second reaction, the product in the four-neck flask was taken out, filtered and washed with suction to obtain 3,5-dichloro-2-acetamidobenzoic acid as a solid. Then add 3,5-dichloro-2-acetamidobenzoic acid solid to 400g of 36.5% (mass concentration, the same below) hydrochloric acid for the third reaction, the reaction temperature is 120°C, liquid chromatogra...

Embodiment 2

[0049] Add 137 g of anthranilic acid and 110 g of acetic anhydride into a 1000 mL four-necked flask, and perform the first reaction at 120° C. to obtain 2-acetamidobenzoic acid. After the first reaction was completed, 500 g of glacial acetic acid was added into the above-mentioned four-necked flask, and after stirring evenly, 150 g of chlorine gas was slowly introduced at 40° C. to carry out the second reaction. After the second reaction, the product in the four-neck flask was taken out, suction filtered and washed to obtain a solid of 3,5-dichloro-2-acetamidobenzoic acid. Then add 3,5-dichloro-2-acetamidobenzoic acid solid into 400g of 36.5% hydrochloric acid to carry out the third reaction, the reaction temperature is 120°C, and the acetic acid generated is continuously distilled during the reaction process to obtain 3,5-dichlorobenzoic acid Chloro-2-aminobenzoic acid. Then the product of the third reaction was added to 120g of isopropanol, 400g of 36.5% hydrochloric acid, ...

Embodiment 3

[0051] Add 137 g of anthranilic acid and 120 g of acetic anhydride into a 1000 mL four-necked flask, and perform the first reaction at 120° C. to obtain 2-acetamidobenzoic acid. After the first reaction was completed, 300 g of glacial acetic acid was added into the above-mentioned four-necked flask, and after stirring evenly, 150 g of chlorine gas was slowly introduced at 40° C. to carry out the second reaction. After the second reaction, the product in the four-neck flask was taken out, suction filtered and washed to obtain a solid of 3,5-dichloro-2-acetamidobenzoic acid. Then add 3,5-dichloro-2-acetamidobenzoic acid solid into 400g of 36.5% hydrochloric acid to carry out the third reaction, the reaction temperature is 130°C, and the acetic acid produced is continuously distilled during the reaction process to obtain 3,5-dichlorobenzoic acid Chloro-2-aminobenzoic acid. Then the product of the third reaction was added to 120g of isopropanol, 400g of 36.5% hydrochloric acid, a...

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Abstract

The invention relates to a preparation method of 3,5-dichlorobenzoyl chloride, and belongs to the field of compound synthesis technology. The preparation method of 3,5-dichlorobenzoyl chloride comprises the following steps: (1) the first reaction: reacting anthranilic acid with acetic anhydride to prepare 2-acetamidobenzoic acid; (2) the second reaction: reacting 2-acetamidobenzoic acid with chlorine to prepare 3,5-dichloro-2-acetamidobenzoic acid; (3) the third reaction: reacting 3,5-dichloro-2-acetamidobenzoic acid with hydrochloric acid to prepare 3,5-dichloro-2-aminobenzoic acid; (4) the fourth reaction: reacting 3,5-dichloro-2-aminobenzoic acid with sodium nitrite, hydrochloric acid and isopropanol to prepare 3,5-dichloro-benzoic acid; (5) the fifth reaction: reacting 3,5-dichloro-benzoic acid with thionyl chloride to obtain the 3,5-dichlorobenzoyl chloride. The preparation method of 3,5-dichlorobenzoyl chloride has protected amino groups prior to chlorination, thereby effectively preventing oxidization of amino groups; and the yield of chlorination is over 95%.

Description

technical field [0001] The invention relates to the technical field of compound synthesis, in particular to a preparation method of 3,5-dichlorobenzoyl chloride. Background technique [0002] 3,5-dichlorobenzoyl chloride is an important pesticide intermediate, its molecular structure is as follows: [0003] . 3,5-Dichlorobenzoyl chloride has a wide range of uses. It can be used to prepare different substances through different reactions. It is mainly used in the production of pesticides, pharmaceuticals, and dyes. In the production of pesticides, 3,5-dichlorobenzoyl chloride can be benzoylated with methionine and its ether in a sodium hydroxide solution environment, and the obtained derivatives can promote plant growth, improve plant conditions, or make pesticides Insecticide. As a pharmaceutical intermediate, different derivatives of 3,5-dichlorobenzoyl chloride can treat different diseases. It reacts with a mixture of tropine and hydrogen chloride to prepare a class o...

Claims

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Application Information

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IPC IPC(8): C07C63/70C07C51/60
CPCC07C51/60C07C51/377C07C227/20C07C231/02C07C231/12C07C63/70C07C229/56C07C233/54
Inventor 孙国庆侯永生朱小猛陈桂元赵广理
Owner SHANDONG RUNBO BIOTECH CO LTD
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