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Method for preparing topramezone intermediate by utilizing supergravity reaction

A hypergravity reactor, the technology of oxaflutole, which is applied in chemical instruments and methods, preparation of organic compounds, chemical/physical/physical-chemical stationary reactors, etc., can solve the problem of low yield in two steps and post-processing Complex, cumbersome work sections, etc.

Active Publication Date: 2021-04-23
利民化学有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the shortcomings of the prior art, such as low two-step yield, cumbersome workshops, and complicated post-treatment, the present invention provides a high-yield, environmentally friendly and suitable for continuous industrial production of benzene prepared by supergravity reaction. The method of metofen intermediate

Method used

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  • Method for preparing topramezone intermediate by utilizing supergravity reaction
  • Method for preparing topramezone intermediate by utilizing supergravity reaction
  • Method for preparing topramezone intermediate by utilizing supergravity reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Embodiment 1 (control test)

[0036] Add 2,3-dimethyl sulfide (10 g, 0.065 mol) and 50 ml of 1,2-dichloroethane into a 250 mL three-necked flask and dissolve with regular stirring, and cool down to 5°C. After cooling down, 48% hydrobromic acid aqueous solution (14.4 g, 0.08 mol) and hydrogen peroxide (22.34 g, 0.197 mol) were added dropwise thereto at the same time, and the temperature was controlled and added dropwise at 5°C. After the dropwise addition, keep warm for 10 minutes, then raise the temperature to 15°C and keep warm for 2 hours. Liquid phase detection reaction. The peak area ratio of 2,3-dimethyl-4-methylsulfonylbromobenzene product is 35.7%, and the peak area ratio of single oxide impurity is 55.1%. Raw materials were not detected.

[0037] This experiment proves that it is difficult to achieve one-pot bromination oxidation of 2,3-dimethyl sulfide under conventional stirring equipment.

[0038] The following is an implementation case of using hypergrav...

Embodiment 2

[0040] Turn on the hypergravity response of the silica material, O 3The gas is metered by the rotameter, and the first gas inlet 1 of the supergravity reaction shell is used to fill the layer along the tangential direction. From the ethylene dichloride solution (50g 2,3-dimethyl sulfide+250ml ethylene dichloride) of the 2,3-dimethyl sulfide of raw material tank 6 after raw material pump 5 metering and from the second gas inlet 3 The hydrobromic acid gas measured by the rotameter enters from the supergravity reaction center together, and the gas-liquid two-phase is mixed at high speed to control the 2,3-dimethyl sulfide, O 3 The molar ratio of feed flow rate and hydrobromic acid gas is 1:6:1.3, the reaction temperature is set at 40°C, and the reaction pressure is 1MP. The rotor speed is 800r / min. The gas after the reaction (containing O 2 ) is drawn through the gas outlet 2, and the liquid after the reaction is thrown out of the packing layer, collected by the shell of the s...

Embodiment 3

[0042] Turn on the hypergravity response of the silica material, O 3 The gas is metered by the rotameter, and the first gas inlet 1 of the supergravity reaction shell is used to fill the layer along the tangential direction. From the ethylene dichloride solution (50g2,3-dimethyl sulfide+250ml ethylene dichloride) of the 2,3-dimethyl sulfide of raw material tank 6 after raw material pump 5 metering and from the second gas inlet 3 The hydrobromic acid gas measured by the rotameter enters from the supergravity reaction center together, and the gas-liquid two-phase is mixed at high speed to control the 2,3-dimethyl sulfide, O 3 The molar ratio of feed flow rate to hydrobromic acid gas is 1:5:1.3, the reaction temperature is set at 40°C, and the reaction pressure is 1MP. The rotor speed is 800r / min. The gas after the reaction (containing O 2 ) is drawn through the gas outlet 2, and the liquid after the reaction is thrown out of the packing layer, collected by the shell of the su...

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Abstract

The invention discloses a method for preparing a topramezone intermediate by utilizing a supergravity reaction, which comprises the following steps of selecting the supergravity reaction, feeding a 2, 3-dimethyl sulfide solution, hydrobromic acid and O3 gas into a supergravity reactor according to a certain proportion flow rate, and carrying out gas-liquid two-phase high-speed mixing, enabling the indissolvable hydrobromic acid and O3 gas to be dispersed in the 2, 3-dimethyl sulfide solution to form a supersaturated solution of nano-scale or micron-scale small bubbles, carrying out a solid-liquid-gas three-phase oxidation bromination one-pot reaction in a rotor containing a catalyst and a filler, and desolventizing the reaction solution to obtain the high-purity 2, 3-dimethyl-4-methylsulfonyl bromobenzene. According to the method, the oxidation bromination two-step reaction of the process realizes one-pot synthesis in the supergravity reaction, and the topramezone intermediate with high yield and high purity is obtained. The method has the advantages of simple operation steps, environmental protection, small equipment size, suitableness for continuous industrial production, high yield and high content of the final product, and production cost reduction.

Description

technical field [0001] The present invention relates to the preparation of intermediates of fine chemical products, in particular to a method for preparing intermediates of fenfentrazone by means of supergravity reaction. Background technique [0002] Topramezone, also known as topramezone, is a new type of highly selective benzyl pyrazolone herbicide with high safety, excellent selectivity, broad-spectrum herbicidal activity, long-term effect and Strong compatibility and other characteristics, the safety is higher than mesotrione and nicosulfuron, it is the safest corn herbicide, and it is also one of the herbicides with the least toxicity to mammals. Fenfentrazone has a novel mechanism of action and belongs to the inhibitors of p-hydroxyphenylpyruvate dioxygenase (HPPD). Grass has a good control effect. Fenfentrazone is mainly used for the control of gramineous weeds and broad-leaved weeds in corn fields. Its main feature is that it is safe for corn and subsequent crops....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/02C07C315/04C07C317/14B01J19/18
Inventor 孙敬权许辉李新生李林虎石卫许宜伟孙丽梅
Owner 利民化学有限责任公司
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