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Synthetic method of 2,3,6-trichlorotoluene

A technology of trichlorotoluene and a synthetic method, which is applied in two fields, can solve the problems of low selectivity, cumbersome preparation methods, and high production costs, and achieve the effects of simple preparation methods, cheap and easy-to-obtain raw materials, and low production costs

Active Publication Date: 2016-05-25
JIANGSU LIANHE CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The technical problem to be solved by the present invention is to overcome the cumbersome preparation method of 2,3,6-trichlorotoluene in the prior art, low yield, low selectivity, poor product purity, expensive raw materials, difficult to obtain, production A kind of synthetic method of 2,3,6-trichlorotoluene is provided due to defects such as high cost and unsuitability for industrialized production

Method used

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  • Synthetic method of 2,3,6-trichlorotoluene
  • Synthetic method of 2,3,6-trichlorotoluene

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Add 100g of 2,6-dichlorotoluene and 0.5g of antimony trichloride into the round-bottomed flask, feed 39.7g of chlorine gas under normal pressure at 25°C, control the reaction temperature at 25-30°C, and pass chlorine at a rate of 10g / h, about Hours later, the GC detection reaction conversion rate was 80%, and the chlorine flow was stopped. 117.6 g of reaction liquid was obtained, and the composition was 20% of 2,6-dichlorotoluene, 77.2% of 2,3,6-trichlorotoluene, 0.7% of 2,4,6-trichlorotoluene, 2.1% of tetrachlorotoluene and impurities. The reaction solution was rectified to obtain 94.6 g of 2,3,6-trichlorotoluene, with a yield of 78.0% (94.6% after recovery of 2,6-dichlorotoluene), and a GC area content of 99%.

Embodiment 2

[0029] Add 100g of 2,6-dichlorotoluene, 100g of 1,2-dichloroethane, 0.5g of antimony trichloride into the round bottom flask, feed 39.7g of chlorine gas under normal pressure at 25°C, and control the reaction temperature at 25-30°C , Chlorine flow rate 10g / h, after about 4 hours, GC detection reaction conversion rate is 80%, stop to pass chlorine. Atmospheric pressure distillation reclaims solvent 1,2-dichloroethane to obtain 117.5 g of still residue, consisting of 20% 2,6-dichlorotoluene, 77.5% 2,3,6-trichlorotoluene, 2,4,6- Trichlorotoluene 0.6%, tetrachlorotoluene and impurities 1.9%. After further rectification, 95.0 g of 2,3,6-trichlorotoluene was obtained, with a yield of 78.3% (94.9% after recovery of 2,6-dichlorotoluene), and a GC area content of 99%.

Embodiment 3

[0031] Add 100g of 2,6-dichlorotoluene and 0.5g of antimony trichloride into the round bottom flask, feed 59.6g of chlorine gas under normal pressure at 25°C, control the reaction temperature at 25-30°C, and pass chlorine at a rate of 10g / h, approx. After 6 hours, GC detected that the reaction of 2,6-dichlorotoluene was complete, and the chlorine flow was stopped. 124.1 g of the reaction solution was obtained, and the composition was 85.4% of 2,3,6-trichlorotoluene, 1.9% of 2,4,6-trichlorotoluene, 12.7% of tetrachlorotoluene and impurities. The reaction solution was rectified to obtain 104.7 g of 2,3,6-trichlorotoluene with a yield of 86.3% and a GC area content of 98%.

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Abstract

The invention discloses a synthetic method of 2,3,6-trichlorotoluene. The invention provides the synthetic method of 2,3,6-trichlorotoluene, wherein the synthetic method includes the following steps: in the presence of a catalyst, 2,6-dichlorotoluene and a chlorination reagent are subjected to a chlorination reaction to obtain 2,3,6-trichlorotoluene, wherein the catalyst is a metal and / or a metal halide. The synthetic method has the advantages of simple preparation method, high yield, high selectivity, high purity of the prepared product, cheap and easy obtained raw materials and low production cost, and is suitable for industrialized production.

Description

technical field [0001] The invention relates to a synthesis method of 2,3,6-trichlorotoluene. Background technique [0002] 2,3,6-Trichlorobenzoic acid, a benzoic acid herbicide, can be used to control some annual and perennial deep-rooted broad-leaved weeds and some shrubs. 2,3,6-Trichlorotoluene is an important intermediate in the synthesis of 2,3,6-trichlorobenzoic acid, and its synthesis has also received extensive attention from chemists. [0003] At present, the methods for synthesizing 2,3,6-trichlorotoluene mainly contain the following: [0004] Patent GB817173A reports a method for preparing 2,3,6-trichlorotoluene from toluene or o-chlorotoluene. When toluene is used as raw material and aluminum trichloride is used as catalyst, the yield of the trichloro mixture is 60%, and the purity of 2,3,6-trichlorotoluene is 60%. When o-chlorotoluene is used as raw material and antimony chloride is used as catalyst, the yield of trichlorotoluene is 77.2%, and the purity of 2...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/12C07C25/02
Inventor 樊小彬林行军徐晓明黄超陈冬辉周述勇
Owner JIANGSU LIANHE CHEM TECH
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