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Preparation method of dichloropentachloromethylthiazole

A technology of dichloropentachloromethylthiazole and chloromethylthiazole, which is applied in organic chemistry and other fields, and can solve problems such as pollution, low product yield, waste of cost, etc.

Pending Publication Date: 2021-06-22
怀仁市普惠生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the process of this synthetic method is simple, it is easy to cause pollution and waste cost by introducing a large amount of chlorine, and the yield of the product is very low, there are many by-products, and the amount of three wastes is large. Therefore, we propose a dichloropentachloromethylthiazole Preparation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Substitution-isomerization reaction

[0029] Add 100g of sodium thiocyanate, 2.5g of tetrabutylammonium bromide and 4g of potassium iodide, and 200mL of water into the three-neck flask, and slowly add 108g of 2,3-dichloropropene with accurate metering dropwise under stirring. Connect the condenser tube, condense and reflux in an oil bath at 80°C for 7 hours, then directly raise the temperature to 115°C for 6 hours (experimental phenomenon: from the original yellow liquid and white solid to dark brown liquid, after high temperature isomerization, it turns into Black opaque liquid), after the reaction was completed and cooled, the solvent water was evaporated on a rotary evaporator to obtain 117.5 g of a black opaque product. Gas chromatographic analysis was carried out to the product and the steamed water, and the product purity was 99.5%, and the yield was 88.3%, and about 4% of the product was contained in the steamed toluene.

[0030] Chlorination-cyclization reactio...

Embodiment 2

[0037] Substitution-isomerization reaction

[0038] Add 100g of sodium thiocyanate, 2.5g of tetrabutylammonium bromide and 4g of potassium iodide, and 200mL of water into the three-neck flask, and slowly add 108g of 2,3-dichloropropene with accurate metering dropwise under stirring. Connect the condenser tube, condense and reflux in an 80°C oil bath for 7 hours, then directly heat up to 110°C for 6 hours (experimental phenomenon: from the original yellow liquid and white solid to dark brown liquid, after high temperature isomerization, it turns into black opaque liquid), after the reaction was completed and cooled, the solvent water was evaporated on a rotary evaporator to obtain 119.3 g of a black opaque product. The product and the steamed water were analyzed by gas chromatography, the product purity was 99.7%, the yield was 88.9%, and the steamed water contained about 3.5% of the product.

[0039] Chlorination-cyclization reaction

[0040] Add the above product 1-isothioc...

Embodiment 3

[0046] Substitution-isomerization reaction

[0047] Add 100g of sodium thiocyanate, 2.5g of tetrabutylammonium bromide and 4g of potassium iodide, and 200mL of water into the three-neck flask, and slowly add 108g of 2,3-dichloropropene with accurate metering dropwise under stirring. Connect the condenser tube, condense and reflux in an 80°C oil bath for 7 hours, then directly raise the temperature to 105°C and react for 6 hours (experimental phenomenon: the original yellow liquid and white solid turn into a dark brown liquid, and after high temperature isomerization, it turns into Black opaque liquid), after the reaction was completed and cooled, the solvent water was evaporated on a rotary evaporator to obtain 117.5 g of a black opaque product. Gas chromatographic analysis was carried out on the product and the water evaporated (gas phase conditions: 55°C for 2min, rising to 250°C at a rate of 20°C per minute), the product purity was 99.5%, and the yield was 88.3%. Contains ...

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PUM

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Abstract

The invention discloses a preparation method of dichloropentachloromethylthiazole, which is characterized in that 2, 3-dichloropropene, sodium thiocyanate, sulfuryl chloride and the like are used as main raw materials, 2-chloro-5-chloromethylthiazole is prepared by changing a reaction solvent, reaction temperature and the like, and the product is purified. According to the preparation method of dichloropentachloromethylthiazole, 2, 3-dichloropropene, ammonium thiocyanate, sulfuryl chloride and the like are used as main raw materials, 2-chloro-5-chloromethylthiazole is prepared by changing a reaction solvent, reaction temperature and the like, and the product is purified. Experimental results show that dichloroethane is used as a solvent, 2, 3-dichloropropene and ammonium thiocyanate are sequentially subjected to a substitution reaction, an isomerization reaction and a chlorination-cyclization reaction through a one-pot process, the 2-chloro-5-chloromethylthiazole can be prepared through simple distillation, the purity can reach 99% or above, and the method is easy to operate, few in side reaction, few in three wastes and high in efficiency.

Description

technical field [0001] The invention relates to the field of preparation of chemical raw materials, in particular to a preparation method of dichloropentachloromethylthiazole. Background technique [0002] The preparation method of existing industrial 2-chloro-5-chloromethylthiazole has two kinds, and the one is toluene as solvent, comprises ammonium thiocyanate, 2,3-dichloropropene is mixed to generate 1-thiocyano- 2-chloropropene, high-temperature isomerization, and sulfuryl chloride are mixed for chlorination. Then add excess hydrochloric acid to convert 2-chloro-5-chloromethylthiazole into hydrochloride and dissolve it in acid water, then extract 2-chloro-5-chloromethylthiazole into the solvent by solvent extraction, and purify by distillation Get 2-chloro-5-chloromethylthiazole product. This technological operation step is complicated, and side reaction is many, and the amount of three wastes is big and difficult to handle, and cost is high, and the 2nd is the chlorof...

Claims

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Application Information

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IPC IPC(8): C07D277/32
CPCC07D277/32
Inventor 荣庆生郭大鹏杨杰吴汝俊
Owner 怀仁市普惠生物科技有限公司
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