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The synthetic method of 2-chlorobenzothiazole

A technology for the synthesis of chlorobenzothiazole and its synthesis method, which is applied in the field of synthesis of 2-chlorobenzothiazole, can solve the problems of high production cost and high risk, and achieve the effects of reducing risk, avoiding pollution, and saving process cost

Active Publication Date: 2019-05-21
甘肃联凯生物科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, due to the use of raw material solid phosgene, the risk in the process is relatively high, and the production cost is relatively high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] In a 500ml reaction bottle, throw 33.4g of 2-mercaptobenzothiazole and 60g of water, add 28.2g of hydrochloric acid with a mass fraction of 30%, raise the temperature to 40°C, add 42g of hydrogen peroxide with a mass fraction of 20%, and after the addition Insulation reaction until HPLC detects that the content of 2-mercaptobenzothiazole in the system is lower than 0.2%, stop adding hydrogen peroxide (about 4 hours of insulation reaction), after the reaction is over, let it stand for stratification, and the upper layer of oily liquid is 2-chlorobenzothiazole. The crude thiazole was finally dried with anhydrous sodium sulfate to obtain 33.1 g of refined 2-chlorobenzothiazole.

Embodiment 2

[0017] In a 500ml reaction bottle, throw 33.4g of 2-mercaptobenzothiazole and 60g of water, add 29.7g of hydrochloric acid with a mass fraction of 30%, raise the temperature to 45°C, add 44.8g of hydrogen peroxide with a mass fraction of 20%, and the addition ends After the heat preservation reaction, when the content of 2-mercaptobenzothiazole in the system detected by HPLC is lower than 0.2%, stop adding hydrogen peroxide (about 4 hours of heat preservation reaction). The crude 2-chlorobenzothiazole was finally dried with anhydrous sodium sulfate to obtain 33.1 g of refined 2-chlorobenzothiazole.

Embodiment 3

[0019] In a 500ml reaction bottle, throw 31.5g of 2-mercaptobenzothiazole and 60g of water, add 28.2g of hydrochloric acid with a mass fraction of 30%, raise the temperature to 35°C, add 43.8g of hydrogen peroxide with a mass fraction of 20%, and the addition ends After the heat preservation reaction, when the content of 2-mercaptobenzothiazole in the system detected by HPLC is lower than 0.2%, stop adding hydrogen peroxide (about 4 hours of heat preservation reaction). The crude 2-chlorobenzothiazole was finally dried with anhydrous sodium sulfate to obtain 31.2 g of refined 2-chlorobenzothiazole.

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PUM

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Abstract

The invention relates to the field of chemical industry, and discloses a synthesis method of 2-chlorobenzothiazole. The method comprises the following steps: (1) dispersing 2-mercaptobenzothiazole in water to form pasty 2-mercaptobenzothiazole; (2) adding 30 wt% hydrochloric acid into the pasty 2-mercaptobenzothiazole, and uniformly mixing to obtain a mixture; (3) heating the mixture to 35-45 DEG C, dropwisely adding an oxidizer, keeping the temperature to react, and stopping dropwisely adding the oxidizer when the 2-mercaptobenzothiazole content detected in the system is lower than 0.2%; and (4) performing standing to stratify, and taking the supernatant oily liquid to obtain the 2-chlorobenzothiazole crude product. Compared with the prior art, the method reduces the discharge quantity of waste gas, lowers the environmental pollution, lowers the hazards in the production process due to no need for hazardous raw materials, and lowers the production cost.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a synthesis method of 2-chlorobenzothiazole. Background technique [0002] There are two main methods for the synthesis of 2-chlorobenzothiazole using 2-mercaptobenzothiazole; [0003] (1) Thionyl chloride chlorination method: Add 2-mercaptobenzothiazole to dichloroethane, add thionyl chloride dropwise at 40°C to 60°C, and react to generate 2-chlorobenzothiazole. A large amount of sulfur dioxide waste gas will be produced in the reaction process of this method, and the environmental pollution is serious. [0004] (2) Phosgene method: Add 2-mercaptobenzothiazole to toluene, and add solid light toluene solution dropwise at about 30°C to generate 2-chlorobenzothiazole. In this method, due to the use of raw material solid phosgene, the risk in the process is relatively high, and the production cost is relatively high. Contents of the invention [0005] Purpose of the invention:...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D333/62
CPCC07D333/62
Inventor 赵飞四董海涛陈宽新黄方利韦东余蒋云翔
Owner 甘肃联凯生物科技有限公司