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Synthetic analysis and detection method for industrially producing p-fluoronitrobenzene

A technology for the synthesis and analysis of p-fluoronitrobenzene, which is applied in the direction of chemical instruments and methods, analytical materials, and the preparation of organic compounds, etc., can solve the problems that the conversion rate and impurity content of fluoronitrobenzene cannot be effectively controlled, and the detection time can be reached Effects of short, high accuracy and sensitivity, and simple operation

Pending Publication Date: 2022-05-13
YUNNAN YUNTIANHUA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a method for the synthesis, analysis and detection of industrial production of p-fluoronitrobenzene, so as to solve the problem that the conversion rate and impurity content in the production process of p-fluoronitrobenzene cannot be effectively controlled in the prior art

Method used

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  • Synthetic analysis and detection method for industrially producing p-fluoronitrobenzene
  • Synthetic analysis and detection method for industrially producing p-fluoronitrobenzene
  • Synthetic analysis and detection method for industrially producing p-fluoronitrobenzene

Examples

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Effect test

Embodiment 1

[0047] (1) Open the feed valve of the fluorination kettle, turn on the vacuum pump to suck in 1500 kg of raw material p-chloronitrobenzene, heat up less than 120° C., dehydrate under negative pressure for 3 hours, until no water is evaporated, and the water content is ≤0.05%. Cool down to 50°C with nitrogen gas, add 2000L of N,N-dimethylformamide (DMF), turn on the vacuum system, and vacuum dehydrate at 90-120°C for about 2 hours at a vacuum of -0.075Mpa. 0.05% qualified, filled with nitrogen to normal pressure, opened the inlet and put in the first batch of potassium fluoride 250kg. After reacting and dehydrating for 2 hours, fill it with nitrogen gas to normal pressure, open the inlet and put in the second batch of potassium fluoride 200kg respectively; after reacting and dehydrating for 2 hours, fill it with nitrogen gas to normal pressure, open the inlet and put in the third batch of potassium fluoride respectively 150kg, turn on the vacuum system, vacuum-0.075Mpa, vacuum ...

Embodiment 2

[0050](1) Open the feed valve of the fluorination kettle, turn on the vacuum pump to suck in 1500 kg of raw material p-chloronitrobenzene, heat up less than 120° C., dehydrate under negative pressure for 3 hours, until no water is evaporated, and the water content is ≤0.05%. Cool down to 50°C with nitrogen gas, add 2000L of N,N-dimethylformamide (DMF), turn on the vacuum system, and vacuum dehydrate at 90-120°C for about 2 hours at a vacuum of -0.075Mpa. 0.05% qualified, filled with nitrogen to normal pressure, opened the inlet and put in the first batch of potassium fluoride 350kg. After reacting and dehydrating for 2 hours, fill it with nitrogen gas to normal pressure, open the inlet and put in the second batch of potassium fluoride 200kg respectively; after reacting and dehydrating for 2 hours, fill it with nitrogen gas to normal pressure, open the inlet and put in the third batch of potassium fluoride respectively 150kg, turn on the vacuum system, vacuum-0.075Mpa, vacuum d...

Embodiment 3

[0053] (1) Open the feed valve of the fluorination kettle, turn on the vacuum pump to suck in 1500 kg of raw material p-chloronitrobenzene, heat up less than 120° C., dehydrate under negative pressure for 3 hours, until no water is evaporated, and the water content is ≤0.05%. Cool down to 50°C with nitrogen gas, add 1500L of N,N-dimethylformamide (DMF), turn on the vacuum system, and vacuum dehydrate at 90-120°C for about 2 hours at a vacuum of -0.075Mpa. 0.05% qualified, filled with nitrogen to normal pressure, opened the inlet and put in the first batch of potassium fluoride 350kg. After reacting and dehydrating for 2 hours, fill it with nitrogen gas to normal pressure, open the inlet and put in the second batch of potassium fluoride 200kg respectively; after reacting and dehydrating for 2 hours, fill it with nitrogen gas to normal pressure, open the inlet and put in the third batch of potassium fluoride respectively 150kg, turn on the vacuum system, vacuum-0.075Mpa, vacuum ...

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Abstract

The invention discloses a synthesis analysis detection method for industrial production of p-fluoronitrobenzene, and relates to the technical field of p-fluoronitrobenzene production. Parachloronitrobenzene is used as a raw material, potassium fluoride and a solvent N, N-dimethylformamide are adopted, under the action of a phase transfer catalyst tetramethylammonium chloride, fluorination is adopted to replace one-step synthesis, reactants are collected in real time in the synthesis process, gas chromatography is used for quantitative analysis, and the content of impurities in the composition is controlled. The method comprises the following steps: dehydrating parachloronitrobenzene, adding N, N-dimethylformamide, and carrying out vacuum dehydration; adding potassium fluoride in batches according to time intervals for dehydration and reaction, adding a phase transfer catalyst tetramethylammonium chloride, and carrying out heating reflux reaction to obtain a crude product p-fluoronitrobenzene; and dissolving the reactant with methanol, filtering, carrying out gas chromatographic analysis, and calculating the conversion rate by adopting a peak area normalization method. The raw materials are subjected to dehydration treatment, the feeding mode, the feeding amount and the reaction time are optimized, and the conversion rate of the reaction is controlled in combination with a gas chromatographic analysis method.

Description

technical field [0001] The invention relates to the technical field of production of p-fluoronitrobenzene, in particular to a method for synthesis, analysis and detection of industrial production of p-fluoronitrobenzene. Background technique [0002] 4-Fluoronitrobenzene (4-Fluoronitrobenzene) is an important intermediate in the preparation of medicines, pesticides, dyes, etc., and is widely used in various fields. "Benben", which is high in toxicity, low in toxicity and high in selectivity, is synthesized with it as the main starting material, and has a high market share. It is mainly made from p-chloronitrobenzene after fluorination. Limited by the current production technology and detection technology level, the actual production of p-fluoronitrobenzene has a low conversion rate of raw materials and often contains p-chloronitrobenzene. If it is directly involved in the subsequent drug synthesis, it will seriously affect the efficacy of the drug. quality and potency. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/68C07C201/12C07C205/12
CPCG01N30/02G01N30/06G01N30/68C07C201/12C07C205/12
Inventor 梁梦洁马航宗世荣万邦隆田强李玉叶蒋兴志雷旭松王君婷
Owner YUNNAN YUNTIANHUA
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