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Synthesis method of mesitylene-2-sulfonyl triazole

A technology for the synthesis of sulfone-triazole and its synthesis method, which is applied in the field of synthesis of mesityl-2-sulfone-triazole, achieving the effects of high purity and simple and easy-to-operate synthesis method

Pending Publication Date: 2022-02-08
宁夏常晟药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Mesityl-2-sulfone triazole is a derivative of triazole, and there is no report on its synthetic method in the prior art, and there is an urgent need for an efficient synthesis of mesityl-2-sulfone Triazole-based method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A synthetic method of mesityl-2-sulfone triazole, comprising the steps of:

[0018] (1) Add 200kg of formamide to the ring closure kettle, start stirring, put in 500kg of thiosemicarbazide, stir for 30 minutes, turn on the jacket steam of the reaction kettle to raise the temperature, raise the temperature to 100°C, keep the heat for 4 hours, and turn on the circulating water to cool down to At 25°C, add 1200kg of methanol, start stirring, add 400kg of potassium hydroxide in batches, control the temperature at 40°C, and stir to obtain 2412kg of compound A;

[0019] (2) Add 700kg of hydrochloric acid into the reaction kettle, then pour in 500kg of water, turn on the frozen brine to cool down, cool down to 3°C, then start to add 500kg of raw material mesitidine, stir for 0.5h, slowly add 300kg of sodium nitrite, drop After completion, keep warm and stir for 2 hours to obtain the diazo solution for use. Check that the metering pumps of the diazo liquid kettle and the potass...

Embodiment 2

[0022] A synthetic method of mesityl-2-sulfone triazole, comprising the steps of:

[0023] (1) Add 200kg of formamide to the ring closure kettle, start stirring, put in 300kg of thiosemicarbazide, stir for 30 minutes, turn on the jacket steam of the reaction kettle to raise the temperature, raise the temperature to 100°C, keep the heat for 4 hours, and turn on the circulating water to cool down to At 25°C, add 1200kg of methanol, start stirring, add 400kg of potassium hydroxide in batches, control the temperature at 40°C, and stir to obtain 2503kg of compound A;

[0024] (2) Add 700kg of hydrochloric acid into the reaction kettle, then pour in 500kg of water, turn on the frozen brine to cool down, and cool down to 3°C, then start to add the raw material mesitylene, stir for 0.5h, slowly add 300kg of sodium nitrite, dropwise completed , insulated and stirred for 2 hours, and the diazo solution was obtained for use. Check that the metering pumps of the diazo liquid kettle and th...

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PUM

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Abstract

The invention belongs to the technical field of chemical intermediates, and particularly relates to a synthesis method of mesitylene-2-sulfonyl triazole. According to the method, formamide, thiosemicarbazide and the like are used as starting raw materials, mesitylene-2-sulfonyl triazole is synthesized through three steps, the synthesis method is simple and easy to operate, and the synthesized product is high in purity.

Description

technical field [0001] The invention belongs to the technical field of chemical intermediates, and in particular relates to a synthesis method of mesityl-2-sulfone triazole. Background technique [0002] Triazole is an organic compound with a chemical formula of CHN. It is widely used in the synthesis of pesticides such as triazole, paclobutrazol, uniconazole, and diniconazole. It is a white needle-like crystal. Industrial products are light yellow or brown needle-like crystals. powerful. Uses It is an intermediate of pesticides and medicines, widely used in the synthesis of pesticides such as triclobutrazol, paclobutrazol, uniconazole, and diniconazole. [0003] Mesityl-2-sulfone triazole is a derivative of triazole, and there is no report on its synthetic method in the prior art, and there is an urgent need for an efficient synthesis of mesityl-2-sulfone method based on triazoles. Contents of the invention [0004] Aiming at the problems of the prior art described abo...

Claims

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Application Information

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IPC IPC(8): C07D249/12
CPCC07D249/12
Inventor 陈健龙金璐仪
Owner 宁夏常晟药业有限公司
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