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Synthesis method of 2-chloro-5-chloromethyl-1,3-thiazole

A synthesis method, chloromethyl technology, applied in electrolysis process, electrolysis components, electrolysis organic production, etc., can solve problems such as equipment corrosion and environmental pollution, achieve the effects of eliminating equipment corrosion, good product purity, and improving atom economy

Inactive Publication Date: 2014-04-23
HARBIN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to solve the problems of equipment corrosion, environmental pollution and personal safety caused by using sulfuryl chloride, chlorine gas, etc. A kind of synthetic method of 2-chloro-5-chloromethyl-1,3-thiazole

Method used

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  • Synthesis method of 2-chloro-5-chloromethyl-1,3-thiazole
  • Synthesis method of 2-chloro-5-chloromethyl-1,3-thiazole
  • Synthesis method of 2-chloro-5-chloromethyl-1,3-thiazole

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specific Embodiment approach 1

[0020] Specific embodiment one: a kind of synthetic method of 2-chloro-5-chloromethyl-1,3-thiazole in this embodiment is carried out according to the following steps:

[0021] 1. Dissolve 1-isothiocyanato-2-chloro-2-propene in an organic solvent, and then mix it with aqueous hydrochloric acid to obtain an electrolyte, wherein the concentration of the aqueous hydrochloric acid is 2.0mol / L to 10.0mol / L; Wherein, the mass volume ratio of 1-isothiocyanato-2-chloro-2-propene to organic solvent is 1g: 3mL~16mL; the ratio of 1-isothiocyanato-2-chloro-2-propene to aqueous hydrochloric acid The mass volume ratio is 1g: 3mL~16mL;

[0022] 2. Place the electrolyte solution prepared in step 1 in a single-chamber electrolytic cell, use platinum sheets as cathode and anode electrodes, and place the electrolyte at a temperature of 0°C to 40°C and a current density of 0.1A / cm 2 ~0.4A / cm 2 Under certain conditions, electrolytic chlorination is carried out, and the electrolytic chlorination t...

specific Embodiment approach 2

[0028] Embodiment 2: This embodiment differs from Embodiment 1 in that: the concentration of hydrochloric acid in step 1 is 2.0 mol / L-8.0 mol / L. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0029] Embodiment 3: This embodiment differs from Embodiment 1 or Embodiment 2 in that: the concentration of hydrochloric acid in step 1 is 2.0 mol / L-4.0 mol / L. Others are the same as in the first or second embodiment.

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Abstract

The invention discloses a synthesis method of 2-chloro-5-chloromethyl-1,3-thiazole. The invention relates to the technical field of organic electrochemistry and aims at the problems of environmental pollution, equipment corrosion, personal safety and the like caused by use of sulfonyl chloride, chlorine and the like as chloride reagents in the synthesis process of 2-chloro-5-chloromethyl-1,3-thiazole. The synthesis method disclosed by the invention comprising the following step: in a single-chamber electrolytic tank, by taking platinum sheets as negative and positive electrodes, 1-isothiocyano-2-chloro-2-propylene as a raw material and a hydrochloric acid solution as electrolyte, carrying out electrolytic chlorination at room temperature to obtain high-purity 2-chloro-5-chloromethyl-1,3-thiazole. According to the synthesis method disclosed by the invention, the chloride reagents are not directly used in production, so that the problems of environmental pollution, personal safety and the like caused by use of the chloride reagents are avoided; chlorination by-product HCl can be recycled as a reaction raw material, so that reaction by-products are reduced, and the atom economy of chlorination reaction is improved; and reaction conditions are mild, the product yield is high, and the purity is high.

Description

technical field [0001] The invention relates to a synthesis method of 2-chloro-5-chloromethyl-1,3-thiazole, which belongs to the technical field of organic electrochemistry. Background technique [0002] Thiamethoxam, Clothianidin and Chlorthiazolin are representative neonicotinoid pesticides, which have become new pesticides at home and abroad because of their systemic, broad-spectrum, high-efficiency, and no cross-resistance with other pesticides. One of the hotspots of development. 2-Chloro-5-chloromethyl-1,3-thiazole is one of the key intermediates in the synthesis of this type of compound, and it is also the most insecticidally active structural part of this type of pesticide molecule. Therefore, the synthesis method of 2-chloro-5-chloromethyl-1,3-thiazole has important practical significance for the development and creation of new, efficient, low dosage and safe new pesticides. [0003] There are many synthetic methods of 2-chloro-5-chloromethyl-1,3-thiazole reported...

Claims

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Application Information

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IPC IPC(8): C25B3/06
Inventor 由君吴绵元刘波郭晓峰张红霞
Owner HARBIN UNIV OF SCI & TECH