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Simple new process method for synthesizing tebuconazole in water phase

A technology of tebuconazole and a new method, applied in the field of water-phase synthesis of tebuconazole, can solve the problems of difficult solvent recovery, long reaction time, loss of product yield and the like, and achieves simple synthesis and post-processing purification process, and the reaction time is convenient. The effect of shortening and high product yield

Inactive Publication Date: 2018-07-20
YANCHENEG HUIHUANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Solvent recovery is difficult, and the product yield loss is serious, which is not conducive to industrial application
It is also reported that by adding PEG and a catalyst, the yield of the final product is improved, but the reaction needs to go through two stages of low temperature and high temperature, the temperature program is more complicated and the reaction time is long, and a large amount of organic solvents are used for the purification of post-treatment products, which is not conducive to environmental protection

Method used

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  • Simple new process method for synthesizing tebuconazole in water phase
  • Simple new process method for synthesizing tebuconazole in water phase
  • Simple new process method for synthesizing tebuconazole in water phase

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 23.8 g of tebuconazole epoxy compound, 120 mL of water, 7.9 g of triazole, 25.2 g of potassium hydroxide, and 0.2 g of tetrabutylammonium chloride into a 500 ml three-necked flask. Warm up to reflux and react for 4h. The normalized content of 4H isomer was determined to be 0.7% by sampling. After cooling down to 10-15° C. and stirring for 1 hour, a large amount of white solid was precipitated, and 30.5 g of the product was obtained after suction filtration and drying, with a yield of 97.4% and a content of 98.1%. The filtrate continued to be applied mechanically to the next batch of synthesis reactions.

Embodiment 2

[0024] Add above-mentioned suction filtration filtrate 143g in the 500ml there-necked flask, then add tebuconazole epoxy compound 23.8g, triazole 7.9g, potassium hydroxide 2.5g. Warm up to reflux and react for 4h. The normalized content of 4H isomer was determined to be 0.5% by sampling. After cooling down to 10-15° C. and stirring for 1 h, a large amount of white solid was precipitated, and 30.4 g of the product was obtained after suction filtration and drying, with a yield of 97.2% and a content of 98.0%. The filtrate can be applied to more than 10 batches.

Embodiment 3

[0026] Add 23.8g of tebuconazole epoxy compound, 160mL of water, 9.4g of triazole, 22.4g of potassium hydroxide, and 4000.5g of polyethylene glycol into a 500ml three-necked flask. Warm up to reflux and react for 3h. The normalized content of 4H isomer was determined to be 1.0% by sampling. After cooling down to 10-15° C. and stirring for 1 hour, a large amount of white solid was precipitated, and 29.7 g of the product was obtained after suction filtration and drying, with a yield of 94.8% and a content of 97.8%.

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Abstract

The invention relates to the field of organic synthesis, in particular to a method for synthesizing tebuconazole in a water phase. In a reported synthesizing method for the tebuconazole, an organic solvent or a fused catalyst is required to promote a reaction; water and the organic solvent are added to perform high-temperature extracting and refining in after-treatment; the process is complicated.According to the method for synthesizing the tebuconazole in the water phase, a finished product, namely, the tebuconazole is obtained by heating to react and cooling to separate out by taking tebuconazole epoxide and triazole as raw materials and taking water as a solvent under the condition of the existence of an alkaline and a catalyst. The water phase obtained by centrifuging is applied continuously; the subsequent reaction yield and the product content are not affected. The method is simple and convenient in process flow, and both the water phase and the catalyst are applied continuously, so that the method has very good application value.

Description

Technical field [0001] The invention relates to a new and simple process for synthesizing tebuconazole in an aqueous phase. Specifically, it is a method that avoids the use of organic solvents, uses water as the solvent for synthesis, and continues to use the aqueous phase and catalyst to increase product yield. Background technique [0002] Tebuconazole is a triazole fungicide introduced to the market by Bayer in 1998. It has excellent biological activity, low dosage, strong systemic properties, and a wide range of applications. In the early days of the launch of tebuconazole, the market developed rapidly, with sales reaching 820 million in 2016, making it one of the top ten fungicide products in the world. [0003] In the last step of the synthesis reaction of tebuconazole, the methods reported in the literature mostly use high-boiling point strong polar solvents as raw materials of epoxy compounds, and then obtain the tebuconazole product after a high-temperature reaction...

Claims

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Application Information

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IPC IPC(8): C07D249/08
CPCC07D249/08Y02P20/584
Inventor 郭建法
Owner YANCHENEG HUIHUANG CHEM
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