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Synthesis method of 2, 4-dichlorobenzyl chloride

A dichlorobenzyl chloride and synthetic method technology, applied in the field of fine chemical organic synthesis, can solve the problems of low conversion rate, high preparation cost, complicated preparation process, etc., and achieve the effect of simplifying the rectification procedure, simplifying the procedure and reducing the cost

Pending Publication Date: 2021-12-03
江苏超跃化学有限公司
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  • Description
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  • Application Information

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Problems solved by technology

[0007] Aiming at the problems in the prior art that the conversion rate is low, the preparation cost of 2,4-dichlorobenzyl chloride is high and the preparation process is complicated, the invention provides a kind of synthetic method of 2,4-dichlorobenzyl chloride, the method is based on 2,4-dichlorotoluene is used as raw material, azobisisobutyronitrile and triethanolamine are used as catalysts, and the conversion rate of 2,4-dichlorotoluene into 2,4-dichlorobenzyl chloride is increased by photochlorination reaction , simplifies the rectification procedure, and at the same time reduces the generation of by-product 2,4-dichlorobenzylidene dichloride, and one-step rectification can achieve the purpose of purifying 2,4-dichlorobenzyl chloride

Method used

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  • Synthesis method of 2, 4-dichlorobenzyl chloride

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Effect test

Embodiment 1

[0021] (1) Heat 16.1g of 2,4-dichlorotoluene to 100°C and add it to the chlorination reaction kettle, add the catalyst 0.016g of azobisisobutyronitrile and 0.012g of triethanolamine, and slowly introduce chlorine gas 8.17g under light conditions g, while raising the temperature to 125°C, reacting for 3.5 hours to generate 2,4-dichlorobenzyl chloride solution, and using a graphite absorber to recover the HCl gas generated during the reaction;

[0022] (2) The 2,4-dichlorobenzyl chloride solution obtained in step (1) was subjected to vacuum distillation, and the product 2,4-dichlorobenzyl chloride 18.96g and 2,4-dichlorobenzylidene dichloride were collected Chlorine 0.30g.

Embodiment 2

[0024] (1) Heat 16.1 g of 2,4-dichlorotoluene to 90°C and put it into the chlorination reaction kettle, add the catalyst 0.013g of azobisisobutyronitrile and 0.0125g of triethanolamine, and slowly introduce chlorine gas at 7.81 g under light conditions g, while raising the temperature to 120°C and reacting for 4 hours to generate 2,4-dichlorobenzyl chloride solution, while using a graphite absorber to recover the HCl gas generated during the reaction;

[0025] (2) The 2,4-dichlorobenzyl chloride solution obtained in step (1) was rectified under reduced pressure, and the product 2,4-dichlorobenzyl chloride 18.86 g and 2,4-dichlorobenzyl chloride were collected. Chlorine 0.35 g.

Embodiment 3

[0027] (1) Heat 16.1 g of 2,4-dichlorotoluene to 80°C and put it into the chlorination reaction kettle, add the catalyst 0.019 g of azobisisobutyronitrile and 0.01 g of triethanolamine, and slowly introduce chlorine gas of 8.0 g under light conditions g, while raising the temperature to 130°C, reacting for 3 hours to generate 2,4-dichlorobenzyl chloride solution, and using a graphite absorber to recover the HCl gas generated during the reaction;

[0028] (2) The 2,4-dichlorobenzyl chloride solution obtained in step (1) was rectified under reduced pressure, and the product 2,4-dichlorobenzyl chloride 18.60 g and 2,4-dichlorobenzyl chloride were collected. Chlorine 0.48 g.

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Abstract

The invention discloses a synthesis method of 2, 4-dichlorobenzyl chloride. The method comprises the following steps: heating 2, 4-dichlorotoluene to 80-100 DEG C, adding catalysts azodiisobutyronitrile and triethanolamine, slowly introducing chlorine under the illumination condition, heating to 120-130 DEG C, reacting for 3-4 hours to generate 2, 4-dichlorobenzyl chloride chlorinated liquid, and carrying out vacuum rectification on the 2, 4-dichlorobenzyl chloride chlorinated liquid to obtain 2, 4-dichlorobenzyl chloride. 2, 4-dichlorotoluene is used as a raw material, azodiisobutyronitrile and triethanolamine are used as the catalysts, through the photochlorination reaction, the conversion rate of converting 2, 4-dichlorotoluene into 2, 4-dichlorobenzyl chloride is increased, the rectification procedure is simplified, meanwhile, generation of a byproduct 2, 4-dichlorobenzylidene dichloride is reduced, the purpose of purifying 2, 4-dichlorobenzyl chloride can be achieved through one-step rectification, procedures are simplified, cost is reduced, and industrial popularization is facilitated.

Description

technical field [0001] The invention belongs to the technical field of fine chemical organic synthesis, and in particular relates to a synthesis method of 2,4-dichlorobenzyl chloride. Background technique [0002] With the improvement of chlorotoluene production capacity and production technology, the production capacity of chlorotoluene gradually appears surplus, and the competitive pressure faced by production enterprises is also increasing. On the other hand, it is necessary to speed up the development of downstream products, and the latter will have a more significant benefit to the enterprise. Therefore, increasing technological innovation and technology research and development capabilities, especially increasing the development and application of downstream fine chemical products has become the main direction for the future development of chlorotoluene products. With the continuous expansion of the downstream product market of chlorotoluene, especially the benzotrifl...

Claims

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Application Information

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IPC IPC(8): C07C17/12C07C17/383C07C25/02B01J31/02
CPCC07C17/12C07C17/383B01J31/0238B01J31/0248C07C25/02
Inventor 任坚跃薛保安殷云武
Owner 江苏超跃化学有限公司
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