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Process for producing 2, 4, 6-trichlorobenzoic acid

A technology of trichlorobenzoic acid and trichlorobenzene, applied in 2 fields, can solve the problems of no price advantage and high price of acylating reagent, and achieve the effects of easy control of reaction conditions, strong price advantage and low production cost

Inactive Publication Date: 2009-05-13
BEIJING ODYSSEY CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of this invention is that the preparation steps are simple, but the disadvantage is that the price of the acylating reagent is relatively high, so that the 2,4,6-trichlorobenzoic acid produced by the invention does not have an advantage in terms of price

Method used

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  • Process for producing 2, 4, 6-trichlorobenzoic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0032] 1. Prepare 2,4,6-trichlorobenzotrichloride by reacting 1,3,5-trichlorobenzene and carbon tetrachloride:

[0033] In a 1000L enamel kettle, put 100kg 1,3,5-trichlorobenzene and 280kg carbon tetrachloride in sequence, stir for 10 minutes, add 100kg anhydrous aluminum trichloride, heat and reflux at 77°C for 8 hours, and release a large amount of hydrochloric acid gas Absorb with water.

[0034] Cool down to 30°C, slowly pump the reaction materials into another 2000L reactor with 300kg of water, stir for 1.5 hours, separate the organic matter in the lower layer, wash the organic matter twice with 2 times the volume of water; then wash the organic layer with 0.3 Steam under MPa pressure was heated for 25 minutes until carbon tetrachloride did not appear. For this reason, the crude product of 2,4,6-trichlorotrichlorotoluene was obtained after recovering carbon tetrachloride.

[0035] 2. Prepare 2,4,6-trichlorobenzoic acid by reacting 2,4,6-trichlorobenzotrichloride with sul...

Embodiment 2

[0042] 1. Prepare 2,4,6-trichlorobenzotrichloride by reacting 1,3,5-trichlorobenzene and carbon tetrachloride:

[0043] In a 1000L enamel kettle, put 274kg1,3,5-trichlorobenzene and 810kg carbon tetrachloride in sequence, stir for 10 minutes, add 300kg anhydrous aluminum trichloride, heat and reflux at 80°C for 10 hours, release a large amount of hydrochloric acid gas and water absorb. Cool down to 40°C, slowly pump the reaction materials into another 2000L reactor with 1000kg of water, stir for half an hour, separate the organic matter in the lower layer, wash the organic matter twice with 2 times the volume of water; then wash the organic layer with 0.3 Steam under MPa pressure was heated for 45 minutes until carbon tetrachloride did not appear. For this reason, 2,4,6-trichlorotrichlorotoluene crude product 250kg was obtained after recovering carbon tetrachloride.

[0044] 2. Prepare 2,4,6-trichlorobenzoic acid by reacting 2,4,6-trichlorobenzotrichloride with sulfuric acid: ...

Embodiment 3

[0051] 1. Add 1,3,5-trichlorobenzene and carbon tetrachloride into the reaction kettle, add anhydrous aluminum trichloride after mixing, reflux at 75°C for 12 hours, 1,3,5-trichlorobenzene The weight ratio of benzene, carbon tetrachloride and anhydrous aluminum trichloride is 1:3.0:1.1; cool down to 45°C, add water 5 times the weight of 1,3,5-trichlorobenzene, stir After 1.5 hours, separate the organic matter in the lower layer; heat the organic matter with steam at a pressure of 0.3 MPa for 45 minutes, and recover carbon tetrachloride to obtain crude 2,4,6-trichlorotrichlorotoluene. The carbon tetrachloride in this step can be reused after being recovered, and the hydrochloric acid gas produced in the reaction process is taken out by an acid-resistant pump and absorbed by water.

[0052] 2. Add water to the reaction kettle, then add concentrated sulfuric acid, heat up to 130°C, add the crude product of 2,4,6-trichlorotrichlorotoluene prepared in step 1 at a rate of 1.6 liters...

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Abstract

The invention relates to a method for preparing 2, 4, 6-trichloro-phenylacetic acid. Specifically, 1,3,5-trichloro-benzene and carbon tetrachloride react to generate 2,4,6-trichloro-benzotrichloride; the 2,4,6-trichloro-benzotrichloride and concentrated sulfuric acid react to prepare the 2,4,6-trichloro-phenylacetic acid; and finally, the 2,4,6-trichloro-phenylacetic acid is formed by refining and crystallization. The preparation method has the advantages of low cost, simple reaction steps, easy control of reaction conditions and the like.

Description

technical field [0001] The invention relates to a preparation method of 2,4,6-trichlorobenzoic acid, in particular to a method for producing 2,4,6-trichlorobenzoic acid through 1,3,5-trichlorobenzene and carbon tetrachloride Methods. Background technique [0002] 2,4,6-Trichlorobenzoic acid is an important pharmaceutical intermediate, which can be used to manufacture immunosuppressants and sensitive reagents for the analysis of leukemia anticancer drugs. [0003] Various methods for synthesizing 2,4,6-trichlorobenzoic acid have been reported in the prior art, and these methods basically use substituted trichlorobenzene as a raw material to prepare 2,4,6-trichlorobenzoic acid. [0004] Patent ZL200410073917.0 discloses a method for preparing 2,4,6-trichlorobenzoic acid by using 1,3,5-trichlorobenzene as a raw material through Friedel-Crafts acylation reaction. The method prepares 1-alkcarbonyl-2,4,6-trichlorobenzene by 1,3,5-trichlorobenzene and an acylating agent through t...

Claims

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Application Information

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IPC IPC(8): C07C63/70C07C51/093
Inventor 吴细兵刘斌
Owner BEIJING ODYSSEY CHEM
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