A post-treatment method of mesotrione reaction product

Abstract

The invention provides a method for post-processing the reaction product of mesotrione, comprising the following steps: (A) acidifying the reaction product of mesotrione, separating to obtain the first organic phase, and crystallizing to obtain the purified product of mesotrione and the mother liquor (B) After adding alkaline solution to the mother liquor for extraction, separate the water phase, acidify the water phase, separate to obtain a second organic phase, and crystallize the second organic phase to obtain a purified product of mesotrione. The post-treatment method of the present invention has high product yield, less three wastes, energy saving and environmental protection, and is suitable for continuous large-scale production.

Description

technical field [0001] The invention relates to the field of post-treatment of mesotrione reaction products, in particular to a post-treatment method of mesotrione reaction products. Background technique [0002] Mesotrione is also known as mesotrione and mesotrione, and its chemical name is 2-(2-nitro-4-thiamphenicolbenzoyl)cyclohexane-1,3-dione, which was developed by Xian Zheng A triketone herbicide developed by DA Corporation. It was launched in Europe in 2001 under the trade name Callisto. Mesotrione is a hydroxypyruvate dioxygenase (HPPD) inhibitor that converts tyrosine to plastoquinone. As a new type of systemic herbicide dedicated to corn fields, mesotrione has the characteristics of broad herbicidal spectrum, high activity, strong miscibility, safety to crops, and strong environmental compatibility. It has great prospects for development and use in my country. [0003] The synthetic reaction of mesotrione is relatively mature, and the synthetic route is: using 4...

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Problems solved by technology

[0005] The post-processing method of transposition rearrangement mainly adopts the following several in the prior art: Patent No. is CN85109771A, CN1860102A in the patent, what all adopt is the method for adding alkali to extract, acidify, add organic solvent to carry out recrystallization, the obtained of these methods The acidified product has a relatively fine particle size and a lot of tar, and the product is easily wrapped by tar. When the lye is made of strong alkali, it is also easy to cause product instability and generate tar

[0006] In addition, the patents with patent numbers CN18530325A and CN105254543A adopt the method of desolventizing the crude product and then recrystallizing it with an alcohol solvent. Recrystallization will easily cause product dissolution loss and reduce the yield, and additionally introduce a solvent different from the reaction system. The system environment is disturbed. In the patent No. WO2018178860A1, the crude product is dissolved with dichloroethane, then partially desolvated, extracted with potassium bicarbonate to the water phase, and then acidified to obtain the product. This method first obtains the crude product and then proceeds The operation of crystallization itself is cumbersome, and the product obtained from acidification has a lot of tar, and the product is easily wrapped in tar

[0007] It can be seen that the post-treatment methods of crude mesotrione in the prior art mostly have problems such as recrystallization causing dissolution loss, low yield, and many by-product tars generated, which have an impact on product purity.

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