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Preparation method of chemical intermediate N-isopropyl p-fluoroaniline

A technology for p-fluoroaniline and isopropyl, which is applied in the field of preparation of chemical intermediate N-isopropyl p-fluoroaniline, can solve the problems of excessive waste water, difficulty in automatic control and the like, and achieves high catalytic activity, simple preparation method and low cost. low effect

Active Publication Date: 2020-04-28
SHANGYU XIES CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, at home and abroad, the synthesis process route of N-isopropyl p-fluoroaniline is relatively mature, mainly depends on the alkylation reagent, which is divided into haloalkane and acetone. Then add haloalkane to react; this route is mature, but it needs to add acid-binding agent dropwise under pressure to control PH, automatic control is difficult, and there is more waste water

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A preparation method of chemical intermediate N-isopropyl p-fluoroaniline, comprising the following steps:

[0028] (1) dissolving cellulose in deionized water to obtain a cellulose solution with a mass concentration of 5%; then freeze-drying the prepared cellulose solution at -5°C for 10 hours to obtain a cellulose aerogel; The prepared cellulose airgel was placed in a muffle furnace, and heat-treated at 700°C under nitrogen protection for 1 hour; after the treatment, it was cooled to room temperature with the furnace to obtain carbonized cellulose aerogel;

[0029] (2) 1.6g nickel acetate and 0.22g hexamethylenetetramine are added to the mixed solvent of 30ml ethanol and ethylene glycol and stirred and mixed to make a mixed solution; then add the cellulose airgel of 10g carbonization treatment; Heating and reacting at 160°C for 6 hours; cooling to room temperature after the reaction, and filtering to obtain nickel-doped carbon aerogel;

[0030] (3) Mix and grind the ...

Embodiment 2

[0034] A preparation method of chemical intermediate N-isopropyl p-fluoroaniline, comprising the following steps:

[0035] (1) dissolving cellulose in deionized water to obtain a cellulose solution with a mass concentration of 10%; then freeze-drying the prepared cellulose solution at -10°C for 15 hours to obtain a cellulose aerogel; The prepared cellulose airgel was placed in a muffle furnace, and heat-treated at 900°C under nitrogen protection for 2 hours; after the treatment, it was cooled to room temperature with the furnace to obtain carbonized cellulose aerogel;

[0036] (2) 1.7g nickel acetate and 0.26g hexamethylenetetramine are added to the mixed solvent of 30ml ethanol and ethylene glycol and stirred and mixed to make a mixed solution; then add the cellulose airgel of 20g carbonization treatment; Heating and reacting at 180°C for 9 hours; cooling to room temperature after the reaction, and filtering to obtain nickel-doped carbon aerogel;

[0037] (3) Mix and grind t...

Embodiment 3

[0041] A preparation method of chemical intermediate N-isopropyl p-fluoroaniline, comprising the following steps:

[0042] (1) dissolving cellulose in deionized water to obtain a cellulose solution with a mass concentration of 6%; then freeze-drying the prepared cellulose solution at -6°C for 11 hours to obtain a cellulose aerogel; The prepared cellulose airgel was placed in a muffle furnace, and heat-treated at 750°C under nitrogen protection for 1.2 hours; after the treatment, it was cooled to room temperature with the furnace to obtain carbonized cellulose aerogel;

[0043] (2) 1.62g nickel acetate and 0.23g hexamethylenetetramine are added to the mixed solvent of 30ml ethanol and ethylene glycol and stirred and mixed to make a mixed solution; then add the cellulose airgel of 12g carbonization treatment; Heating and reacting at 165°C for 6.5 hours; cooling to room temperature after the reaction, and filtering to obtain nickel-doped carbon aerogel;

[0044](3) Mix and grind...

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Abstract

The invention discloses a preparation method of a chemical intermediate that is N-isopropyl p-fluoroaniline, which is characterized in that the method comprises adding p-fluoronitrobenzene, a hydrogenation catalyst and acetone into a reaction kettle, heating to 55-75 DEG C, and introducing hydrogen into the reaction kettle to perform hydrogenation reduction reaction; after the reaction is finished, filtering the reaction system to recover the waste catalyst, and layering the filtrate obtained by filtering to obtain wastewater; and then performing rectification to obtain the target product N-isopropyl p-fluoroaniline; the hydrogenation catalyst is a composite catalyst, and the composite catalyst takes a nickel-doped carbon aerogel / TiO2 composite material as a carrier and Pt as a catalytic active component. The method disclosed by the invention is simple in process, economical, environment-friendly and high in product yield.

Description

Technical field: [0001] The invention relates to the field of organic synthesis, in particular to a method for preparing a chemical intermediate N-isopropyl-p-fluoroaniline. Background technique: [0002] N-isopropyl p-fluoroaniline, the pure product is a colorless liquid, the industrial product is a light yellow to yellow liquid, the melting point is -20°C, the boiling point is 217°C, it is stored under airtight conditions, insoluble in water, soluble in various organic solvent. The molecular structure of N-isopropyl-p-fluoroaniline can be regarded as a derivative in which the hydrogen in the ammonia molecule is replaced by isopropyl and fluorobenzene, similar to inorganic ammonia, in which the N atom is sp3 hybridized, and there is a lone pair of electrons on the N atom , which embodies a series of chemical properties, such as easy neutralization, acylation, sulfonation and other reactions on the amino group, and a series of useful compounds are synthesized. N-isopropyl ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/52C07C209/00C07C209/84
CPCC07C209/00C07C209/84C07C211/52Y02P20/584
Inventor 解卫宇卢晓健
Owner SHANGYU XIES CHEM IND
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