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A kind of cleaning preparation method of tebuconazole

A tebuconazole and clean technology, applied in the field of clean preparation of tebuconazole, can solve problems such as low reaction yield, inability to realize clean preparation of tebuconazole, difficult recovery of reaction solvent, etc., and achieve simple and easy post-processing, high The effect of industrial application value

Active Publication Date: 2020-09-18
SHANGHAI SHENGNONG PESTICIDE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the process is complicated to operate, and the obtained tebuconazole product must be refined twice, resulting in an excessive amount of "three wastes"
[0008] This shows that most of the tebuconazole synthesis techniques provided in the prior art have technical defects in many engineering and process aspects, such as low reaction yield, secondary refining of the resulting product, and difficult recovery of the reaction solvent. Realize the clean preparation of tebuconazole

Method used

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  • A kind of cleaning preparation method of tebuconazole
  • A kind of cleaning preparation method of tebuconazole
  • A kind of cleaning preparation method of tebuconazole

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preparation example Construction

[0028] In a preferred embodiment, the cleaning preparation method of tebuconazole comprises the following specific steps:

[0029] S1: Add 1,2,4-triazole, potassium hydroxide, diethylene glycol monomethyl ether into a reaction vessel, after heating, slowly add the reaction material A dropwise, and then keep warm for reaction;

[0030] S2: After the reaction is complete, let stand to cool, filter with suction, take the filter cake, wash the filter cake with n-hexane, and dry to obtain the target product tebuconazole.

[0031] In a further preferred embodiment, the molar amount of the potassium hydroxide is 0.1-1.5 times the molar amount of the reaction raw material A.

[0032] In a further preferred embodiment, the mass of the diethylene glycol monomethyl ether is 0.5-10.0 times the mass of the reaction raw material A.

[0033] In a further preferred embodiment, the duration of slowly adding the reaction material A dropwise is 0.5-5 hours.

[0034] In a further preferred embo...

Embodiment 1

[0044] Add 20.5g of 1,2,4-triazole, 100.0g of diethylene glycol monomethyl ether and 6.5g of potassium hydroxide to a 500ml three-necked flask, heat in an oil bath, and control the internal temperature at 100-105°C; Then, slowly add 60.0 g of the reaction material A dropwise, and the dropping time is 2 hours. After the drop is completed, keep stirring at 100-110° C. for 10 hours. TLC monitors that the reaction of the reaction material A is complete. Then, the reaction solution was allowed to stand and cooled to room temperature, kept in an ice-water bath for 1 h, suction filtered, and the mother liquor collected by suction filtration was used mechanically, and the filter cake was taken, rinsed with 50ml of n-hexane, and vacuum-dried to obtain 67.9 g of tebuconazole product quality, The purity is 98.0%, and the total yield is 91.0%. The tebuconazole product is characterized as follows: GCMS (M+): 307.2[6], 274.1[6], 250.1[100], 207.1[11], 163.1[14], 125.1[100], 103.1[12], 83.1[...

Embodiment 2

[0046]Add 21.0g of 1,2,4-triazole, 150.0g of diethylene glycol monomethyl ether and 7.0g of potassium hydroxide to a 500ml three-necked flask, heat in an oil bath, and control the internal temperature at 100-110°C; Then, slowly add 60.0 g of the reaction material A dropwise, and the dripping duration is 1 hour. After the drop is completed, keep stirring at 100-120° C. for 10 hours. TLC monitors that the reaction material A is completely reacted. Then, the reaction solution was allowed to stand and cooled to room temperature, kept warm in an ice-water bath for 1 hour, suction filtered, and the mother liquor collected by suction filtration was used mechanically, and the filter cake was taken, rinsed with a mixed solvent of 50ml of n-hexane and petroleum ether, and vacuum-dried to obtain tebuconazole The quality of the alcohol product is 68.6g, the purity is 98.2%, and the total yield is 92.1%. The tebuconazole product characterization data are the same as in Example 1.

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Abstract

The invention belongs to the technical field of organic synthesis and specifically relates to a clean preparation method of tebuconazole. The clean preparation method comprises the following steps: S1: adding 1,2,4-triazole, inorganic alkali and diethylene glycol monomethyl ether serving as a solvent into a reaction vessel, carrying out heating, slowly and dropwise adding a reaction raw material A, and then, carrying out a heat preservation reaction; S2, carrying out a complete reaction, then, carrying out standing and cooling, and then, carrying out aftertreatment to obtain tebuconazole serving as a target product. In the clean preparation method of tebuconazole, a mother solution obtained by aftertreatment can be further applied to the next batch of reaction solution, but the reaction yield and the conversion rate of the reaction raw material A are not affected; and therefore, the solvent is not needed to be recovered, and the aftertreatment is simple and easy. In addition, the totalyield of the clean preparation method of tebuconazole reaches 91% or above, and the purity of a tebuconazole product reaches 98%, and therefore, tebuconazole shows a relatively high industrial application value.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a clean preparation method of tebuconazole. Background technique [0002] Tebuconazole is a triazole fungicide developed by Bayer in 1986. The structural formula of tebuconazole is as follows: [0003] [0004] It is an ergosterol demethylation inhibitor, which has three functions of protection, treatment and eradication, and has high efficiency, low toxicity and broad-spectrum characteristics. It not only has high activity, but also has a long-lasting effect. It is mainly used for seed treatment and foliar spray on crops such as wheat, vegetables, bananas, and apples. It is an ideal fungicide at present and has broad application prospects, so it has received widespread attention. [0005] As of December 2016, a total of 51 tebuconazole technical products, 284 single doses and 234 mixtures have been registered in my country. Judging from the current re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D249/08
Inventor 叶振君王涛徐海燕毕强韩海平
Owner SHANGHAI SHENGNONG PESTICIDE
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