Flufenacet preparation method

The technology of flufenacet and flufenamide is applied in the field of preparation of flufenox, which can solve the problems of low synthesis efficiency of flufenox, low purity of flufenox and high requirements on reaction conditions, and achieves reduction of production cost, The effect of reducing side reactions and increasing the reaction rate

Inactive Publication Date: 2018-02-23
江苏绿叶农化有限公司
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Problems solved by technology

At present, the synthesis efficiency of flufenacet is low, the yield is low, and the reaction conditions are high, the environmental pro

Method used

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Embodiment 1

[0029] Such as figure 1 with figure 2 , a preparation method of flufenacet, comprising the following steps:

[0030] Step (1): Synthesis of 2,2-methylthio-5-trifluoromethyl-1,3,4-thiadiazole

[0031] Pump 3 mol of trifluoroacetic acid into the trifluoroacetic acid metering tank for use, then add 1 mol of thiohydrazine and toluene into the synthesis kettle, stir and cool to 10-20°C, start to add trifluoroacetic acid dropwise, and control the temperature during the dropping process to 10-20°C 20°C, after the dropwise addition, stir the reaction at room temperature for 2 hours. After the reaction, then distill. After the distillation, a colorless liquid is obtained, that is, 2,2-methylthio-5-trifluoromethyl-1,3, 4-thiadiazole (TLC and the reference substance showed the same Rf value); yield (93%, purity 96%).

[0032]

[0033] Step (2): Synthesis of 2-thiamphenicol-5-trifluoromethyl-1,3,4-thiadiazole

[0034] Add sodium persulfate to the reaction kettle of step (1) 2,2-me...

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Abstract

The invention discloses a flufenacet preparation method, which comprises synthesis of 2-methylsulfonyl-5-trifluoromethyl-1,3,4-thiadiazole, synthesis of 2-hydroxy-N-(4-fluoroaniline)-N-(1-methylethyl)acetamide and synthesis of 4'-fluoro-N-isopropyl-2-[5-(trifluridine)-1,3,4-thiadiazole-2-imide]acetamide. The optimal flufenacet preparation method is screened by a large number of experiments, the whole process is reasonable in design, particularly the steps of screening optimal reaction conditions and the optimal amount ratio, reaction temperature, reaction time and the like of reaction raw materials, the reaction yield (capable of reaching 90 percent or more) can be greatly increased, side reaction can be reduced, the reaction rate can be increased, the reaction raw materials can be recycled, the production cost is greatly reduced, and a broad application prospect is achieved.

Description

technical field [0001] The invention belongs to the technical field of synthetic chemistry, and in particular relates to a preparation method of flufenacet. Background technique [0002] Flufenacet, Chinese name 4-fluoro-N-isopropyl-2-[5-(trifluoroglycoside)-1,3,4-thiadiazo-2-imine]acetamide, CAS registration number is 142459-58-3, Agrochemicals A. At present, the synthesis efficiency of flufenacet is low, the yield is low, and the reaction conditions are high, the environmental protection is poor, and the purity of the synthesized flufenacet is low, the cost is high, and the industrial promotion is difficult. Contents of the invention [0003] Purpose of the invention: the purpose of the invention is to overcome the deficiencies of the prior art, to provide a kind of process design is reasonable, easy to operate, especially high synthesis efficiency, high yield, less waste, can realize recycling, low cost, high purity The preparation method of flufenacet. [0004] Tech...

Claims

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Application Information

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IPC IPC(8): C07D285/13
CPCC07D285/13
Inventor 彭荣贵陈标乐成芝裴建华
Owner 江苏绿叶农化有限公司
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