Clean and environment-friendly production process of 2-chloro-5-chloromethylthiazole

A chloromethylthiazole, clean and environmentally friendly technology, applied in the direction of organic chemistry, etc., can solve the problems of alkali consumption, high yield and purity, no guidance scheme is given, and achieves the effect of solving environmental pollution, high yield and purity

Inactive Publication Date: 2020-10-16
河北硕俊生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problem of route (4) is to neutralize the hydrogen chloride in 2-chloro-5-chloromethylthiazole hydrochloride, which needs to consume a large amount of alkali and produce a large amount of saline waste water, which increases a lot for the subsequent waste water treatment. large processing costs
[0008] The above technologies have not provided specific guidance on how to make the production process of 2-chloro-5-chloromethylthiazole mild in reaction conditions, low in toxicity, high in yield and purity, and environmentally friendly.

Method used

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  • Clean and environment-friendly production process of 2-chloro-5-chloromethylthiazole
  • Clean and environment-friendly production process of 2-chloro-5-chloromethylthiazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: the production technology (production method) of the clean and environment-friendly 2-chloro-5-chloromethylthiazole of the present invention comprises the following processing steps: 1. 1mol sodium thiocyanate is dissolved in 160g in 1000ml four-necked bottle In water, the mass ratio of sodium thiocyanate to water is 1:1.975, add 2,3-dichloropropene dropwise in a four-necked bottle at 70°C, and the feeding moles of 2,3-dichloropropene and sodium thiocyanate The ratio is 1.1:1, the dropping time is 6 hours, after the dropping is completed, the heat preservation reaction is 6 hours, and the obtained material is washed and layered with water, and the intermediate product 2-chloropropenyl isothiocyanate is obtained by distillation, which is set aside; ② in a 1000ml four-necked bottle Dissolve the intermediate product 2-chloropropenyl isothiocyanate in 300g of dichloroethane, the mass ratio of 2-chloropropenyl isothiocyanate to dichloroethane is 1:2.36, at 50°C ...

Embodiment 2

[0023] Embodiment 2: the production technique of the clean and environment-friendly 2-chloro-5-chloromethylthiazole of the present invention comprises following processing steps: 1. in 1000ml four-necked bottle, 1mol sodium thiocyanate is dissolved in 178g water, thiocyanate The mass ratio of sodium thiocyanate to water is 1:2.2, and 2,3-dichloropropene is added dropwise in a four-necked bottle at 90°C, and the molar ratio of 2,3-dichloropropene to sodium thiocyanate is 1.2: 1. The dropping time is 4.5 hours. After the dropping is completed, keep warm for 5 hours. The obtained material is washed with water, stratified, and distilled to obtain the intermediate product 2-chloropropenyl isothiocyanate, which is set aside; The product 2-chloropropenyl isothiocyanate is dissolved in 350g of dichloroethane, the mass ratio of 2-chloropropenyl isothiocyanate and dichloroethane is 1:2.8, at 55°C in four ports 0.97mol sulfonyl chloride was added dropwise in the bottle for the first time...

Embodiment 3

[0024] Embodiment 3: the production technology of the clean and environment-friendly 2-chloro-5-chloromethylthiazole of the present invention comprises following processing steps: 1. in 1000ml four-necked bottle, 1mol sodium thiocyanate is dissolved in 145g water, thiocyanate The mass ratio of sodium thiocyanate to water is 1:1.8, and 2,3-dichloropropene is added dropwise in a four-necked bottle at 100°C, and the molar ratio of 2,3-dichloropropene to sodium thiocyanate is 1.2: 1. The dropping time is 8 hours. After the dropping is completed, keep warm for 6 hours. The obtained material is washed with water, stratified, and distilled to obtain the intermediate product 2-chloropropenyl isothiocyanate, which is set aside; ② Put the intermediate product in a 1000ml four-necked bottle Dissolve 2-chloropropenyl isothiocyanate in 399g of dichloroethane, the mass ratio of 2-chloropropenyl isothiocyanate to dichloroethane is 1:3, in a four-necked bottle at 60°C 1mol sulfonyl chloride w...

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Abstract

The invention relates to a clean and environment-friendly production process of 2-chloro-5-chloromethylthiazole, which comprises the following steps: dissolving sodium thiocyanate in water, dropwiselyadding 2, 3-dichloropropene, carrying out heat preservation reaction after the dropwisely adding is completed, washing the obtained material with water, layering, and distilling to obtain an intermediate product 2-chloropropenyl isothiocyanate; dissolving the intermediate product in dichloroethane, dropwise adding sulfonyl chloride for the first time at the temperature of 30-60 DEG C, carrying out heat preservation reaction after dropwise adding is finished, degassing, desolventizing and cooling the obtained material, dropwise adding sulfonyl chloride for the second time, carrying out heat preservation reaction after dropwise adding for the second time, adding a stabilizer into the obtained material, and distilling to obtain 2-chloro-5-chloromethylthiazole. According to the invention, a pure byproduct sodium chloride is obtained, and the problem of high ammonia-nitrogen wastewater is solved. Due to the fact that the sulfonyl chloride is appropriate in use amount and is added in two times, by-products of sulfur dioxide and hydrogen chloride gas are reduced, the problem of environmental pollution is solved, and the production process is mild in reaction condition, small in toxicity,high in yield and purity and environmentally friendly.

Description

technical field [0001] The invention relates to a production process of 2-chloro-5-chloromethylthiazole, in particular to a clean and environment-friendly production process of 2-chloro-5-chloromethylthiazole. Background technique [0002] The English name of 2-chloro-5-chloromethylthiazole is: 2-Chloro-5-Chloromethylthiazole, CAS registration number: 105827-91-6, molecular formula is: C 4 h 3 Cl 2 NS, molecular weight: 168.0443, structural formula is as follows: [0003] [0004] 2-Chloro-5-chloromethylthiazole is a key intermediate for the synthesis of highly effective insecticides thiamethoxam and clothianidin. Thiamethoxam and Clothianidin are a new generation of chlorinated nicotinic insecticides. They are strong systemic insecticides and are the receptors of nicotinic acid acetylcholinesterase. They are used to control sucking mouthparts pests , such as aphids, leaf-chan, planthoppers, thrips, whitefly and their resistant strains. At the same time, the toxicity ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/32C07D417/06
CPCC07D277/32C07D417/06
Inventor 肖馥敏
Owner 河北硕俊生物科技有限公司
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