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Flonicamid intermediate synthesis method

A technology of flonicamid and a synthesis method, which is applied in the field of synthesizing flonicamid intermediates, can solve the problem of low product conversion rate and the like, and achieves the effects of reducing reaction time and energy consumption, reducing reaction time and reaction safety.

Inactive Publication Date: 2020-02-11
ANHUI JINGHE IND
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Problems solved by technology

[0003] The purpose of the present invention is to provide a synthetic method of flonicamid intermediate (trifluoroacetoxy vinyl ethyl ether) in order to solve the problem of low product conversion rate in the existing production technology

Method used

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  • Flonicamid intermediate synthesis method

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Embodiment 1

[0014] (1) Add 800 L of dichloromethane and 290 Kg of pyridine into the reactor, cool down to -5°C, and then add 205 Kg of trifluoroacetic acid dropwise, during which the temperature of the reactor is controlled at -5°C~0°C;

[0015] (2) Continue to drop 130 Kg of vinyl ether into the reactor, and control the temperature drop of the reactor at -5°C~0°C

[0016] (3) Subsequently, 208 Kg of methanesulfonyl chloride was added dropwise to reduce the binding energy of the C-O bond;

[0017] (4) Control the reaction temperature at 12°C, and react for 4 hours to generate trifluoroacetoxy vinyl ethyl ether, an intermediate of flonicamid;

[0018] (5) Add trifluoroacetoxy vinyl ether and 650 L of water into the reaction kettle, wash the trifluoroacetoxy vinyl ether with water, keep the lower organic phase, and discard the water phase for three-waste treatment;

[0019] (6) Add 650 L of 2% phosphoric acid and 950 L of organic phase into the reaction kettle, wash with phosphoric acid, d...

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Abstract

The invention relates to a flonicamid intermediate synthesis method, which comprises: (1) adding dichloromethane and pyridine into a reaction kettle, controlling a mass ratio of dichloromethane to pyridine at 4-5:1, cooling to below 10 DEG C, adding trifluoroacetic acid in a dropwise manner, and controlling a mass ratio of trifluoroacetic acid to pyridine at 0.7-0.8: ; (2) cooling the reaction kettle to less than -5 DEG C, adding ethyl vinyl ether in a dropwise manner, and controlling a mass ratio of ethyl vinyl ether to pyridine at 0.4-0.5:1; (3) cooling the reaction kettle to below -5 DEG C,adding methylsulfonyl chloride in a dropwise manner, controlling a mass ratio of methylsulfonyl chloride to pyridine at 0.7-0.8:1, and reacting at 10-15 DEG C for 2-4 h to generate a flonicamid intermediate trifluoroacetic acid ethyl vinyl ether; and (4) washing sequentially with water and 2% phosphoric acid. According to the invention, by adjusting the dropwise adding sequence of ethyl vinyl ether, the temperature of the early reaction is increased, the energy consumption is reduced, the reaction time is shortened, and the yield is increased; and the reaction is carried out in a normal-pressure state and is safe.

Description

technical field [0001] The invention belongs to the technical field of chemical production, relates to the technical field of flonicamid production, in particular to a method for synthesizing a flonicamid intermediate. Background technique [0002] Flunicamid is a new type of low-toxic pyridine amide insect growth regulator insecticide. Under the national policy of replacing phosphorus-containing and highly toxic pesticides, the market prospect is very broad. At present, the production of trifluoroacetate vinyl ether In the process, there are problems of low reaction temperature, high energy consumption, and low conversion rate. Therefore, the technical research and optimization of this product is of great significance to the development of enterprises and local economies. Contents of the invention [0003] The purpose of the present invention is to solve the problem of low product conversion rate in the existing production technology, and to provide a synthesis method of ...

Claims

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Application Information

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IPC IPC(8): C07C45/45C07C45/80C07C49/255C07C51/60C07C53/48
CPCC07C45/455C07C45/80C07C51/60
Inventor 杨志健祁飞耿庆保易健康
Owner ANHUI JINGHE IND
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