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Preparation method of o-fluoroaniline

A technology of o-fluoroaniline and o-fluoronitrobenzene, which is applied in the field of preparation of o-fluoroaniline, can solve problems affecting product yield, achieve the effects of increasing yield and purity, improving reaction efficiency, and reducing defluorination rate

Inactive Publication Date: 2017-09-01
SHANGYU XIES CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the process of catalytic reduction, it is often accompanied by the progress of dehalogenation reaction, which affects the yield of the product.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Fill the continuous reactor with water, replace it with nitrogen for 3 times, then raise the temperature to 80°C, add 150kg of o-fluoronitrobenzene into the reactor every hour, and mix 1.0kg of catalyst, 0.01kg of hypophosphorous acid and 550kg of water at the same time Add it into the continuous reactor after uniformity, and feed 12kg of hydrogen into the continuous reactor at the same time to ensure the pressure of 2.0MPa, and keep feeding continuously. After 24 hours, the reaction ends, and the product passes through the layered tank. Layers can be reused and the lower layer is the product. After testing, the yield of the product was 99.0%, and the percentage content of the dehalogenated product was 0.02%.

Embodiment 2

[0027] Fill the continuous reactor with water, replace it with nitrogen for 3 times, then raise the temperature to 80°C, add 150kg of o-fluoronitrobenzene into the reactor every hour, and mix 2.0kg of catalyst, 0.03kg of hypophosphorous acid and 550kg of water at the same time Add it into the continuous reactor after uniformity, and feed 12kg of hydrogen into the continuous reactor at the same time to ensure the pressure of 2.0MPa, and keep feeding continuously. After 24 hours, the reaction ends, and the product passes through the layered tank. Layers can be reused and the lower layer is the product. After testing, the yield of the product was 99.06%, and the percentage content of the dehalogenated product was 0.02%.

Embodiment 3

[0029] Fill the continuous reactor with water, replace it with nitrogen for 3 times, then raise the temperature to 80°C, add 150kg of o-fluoronitrobenzene into the reactor every hour, and mix 1.2kg of catalyst, 0.02kg of hypophosphorous acid and 550kg of water at the same time Add it into the continuous reactor after uniformity, and feed 12kg of hydrogen into the continuous reactor at the same time to ensure the pressure of 2.0MPa, and keep feeding continuously. After 24 hours, the reaction ends, and the product passes through the layered tank. Layers can be reused and the lower layer is the product. After testing, the yield of the product was 99.06%, and the percentage content of the dehalogenated product was 0.02%.

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Abstract

The invention discloses a preparation method of o-fluoroaniline, which relates to the field of organic synthesis, and specifically comprises the following steps: in a continuous reactor, the system is filled with water, and after three times of nitrogen replacement, the temperature is raised to 80°C, and the system is simultaneously pumped Put in o-fluoronitrobenzene, catalyst, inhibitory dehalogenation agent, water, (catalyst, inhibitory dehalogenation agent and water are mixed, stir evenly and pour in together) and hydrogen gas is introduced at the same time to ensure a pressure of 2.0MPa. Keep feeding continuously, the product is stratified through the stratified tank, and the product is obtained from the lower layer. Apply to the upper water layer. The preparation method disclosed by the invention is suitable for continuous large-scale production of o-fluoroaniline, has simple operation, high product purity and high yield, and the percentage content of the dehalogenated product is reduced to 0.02%.

Description

[0001] Technical field: [0002] The invention relates to the field of organic synthesis, in particular to a preparation method of o-fluoroaniline. [0003] Background technique: [0004] O-fluoroaniline is an important intermediate in the synthesis of fluorine-containing medicines and dyes. O-fluoroaniline can be used to synthesize thermosensitive dye FH-102, which is a kind of thermosensitive dye with wide application and excellent performance to show black color. The dye can be used in the production of computer terminal output printing paper, electrocardiogram recording paper, telephone fax paper and transparent heat-sensitive film for oil fields. [0005] In China, o-fluoroaniline is mainly produced by reducing o-fluoronitrobenzene with iron powder. This process will produce a large amount of iron sludge and a large amount of amine-containing wastewater, which will cause great harm to the environment. Therefore, catalytic hydrogenation reduction is used. The synthesis me...

Claims

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Application Information

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IPC IPC(8): C07C209/36C07C211/52
CPCC07C209/365C07C211/52
Inventor 解卫宇顾临江高益民柳衍森
Owner SHANGYU XIES CHEM IND
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