47 results about "P-fluoronitrobenzene" patented technology

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.

A triarylamine-containing oxazine polymer and a preparation method and application thereof are disclosed. The invention relates to a triarylamine-containing oxazine polymer and a preparation method and application thereof. The invention is to solve the problem that the conventional triarylamine-based polymer has poor heat resistance and an electrochromic polymer film has poor film attaching ability. According to the invention, N,N'-di-naphthyl-1,4-phenylenediamine, which is used as a raw material, reacts with p-fluoronitrobenzene to realize nitration, and then nitro group is reduced to an amino group; and bisphenol A, paraformaldehyde and the prepared triphenylamine-based monomer are used as raw materials to undergo a condensation reaction under a certain conditions to synthesize a polymer. The polymer has excellent electrochromic property and memory performance, can be applied in the field of electrochromism, and also performs well in explosives detection. The invention is applied inthe field of electrochromic polymers.

The invention provides a method for producing p-fluoroaniline by a solvent-free catalytic hydrogenation method. The method comprises that p-fluoronitrobenzene as a raw material undergoes a catalytic hydrogenation reaction in an autoclave under the condition of no solvent and use of a catalyst and a phosphate to produce p-fluoroaniline. The method utilizes a solvent-free hydrogenation method. Compared with the existing solvent hydrogenation method, the method greatly increases reaction efficiency, obviously improves the equipment utilization rate, effectively prevents the energy consumption andequipment cost caused by the solvent recovery, belongs to the pollution-free environment-friendly processes and effectively prevents the production of a large amount of wastewater and waste slag. Thenoble metal catalyst Pt / C is prepared through simple processes and can be recycled in the catalyst reaction and the metal in the catalyst can be recovered and recycled so that the production cost isfurther reduced. The phosphate can be used as a dehydrogenation inhibitor and can improve a reaction conversion rate.

The invention discloses a viologen derivative electrochromic and electrofluorescent discoloration bifunctional material as well as a preparation method and application thereof. The preparation method comprises the following steps: by taking 4, 4 '-dipyridyl as a raw material, carrying out nucleophilic substitution reaction on the 4, 4'-dipyridyl and 1-chloro-2, 4-dinitrobenzene to generate Zincke salt; carrying out nucleophilic substitution reaction on p-fluoronitrobenzene and a nitrogen-containing aromatic heterocyclic ring to generate a nitro compound, and reducing the nitro compound into an amino compound by using hydrazine hydrate as a reducing agent; and performing Zincke reaction on products of the two-step reaction to generate a target product. According to the invention, a benzimidazole group with an electron donating effect is introduced into a viologen derivative, and forms an electron donating-electron withdrawing effect with an electron-deficient bipyridine group, so that the color change voltage is reduced, and the optical contrast is improved; meanwhile, an electrofluorescence discoloration function is introduced into the viologen derivative.

The invention discloses a method for preparing 4-nitrotriphenylamine, which comprises the following steps that: diphenylamine and alkali are reacted in an organic solvent, then fluoronitrobenzene is added into the organic solvent; and the product is obtained by reaction at 10 to 30 DEG C; and the organic solvent is one or more of dimethyl sulfoxide, N, N-dimethyl acetamide, dimethylimidazolidinone and methylpyrrolidone. The method preferably selects the solvent to ensure that the reaction can be performed at room temperature and has no byproducts, is simple and effective, has low cost, convenient use of raw materials, short reaction time and high yield, and is easy to apply to industrialized production.

The invention discloses a 2,4,4'-tribromodiphenyl ether hapten preparation method and application thereof. 2,4-dibromophenol and 4-fluoronitrobenzene are used as raw materials for electrophilic substitution reaction to synthesize 4-nitro-2',4'-dibromodiphenyl ether, and then through hydrogenation reduction reaction, a 2,4,4'-tribromodiphenyl ether hapten is prepared. By means of the method, the problem is solved that the 2,4,4'-tribromodiphenyl ether does not have an active group coupled to carrier protein, the method is simple, the speed is high, the yield is higher, the synthesized 2,4,4'-tribromodiphenyl ether hapten can be used for preparing a 2,4,4'-tribromodiphenyl ether artificial coating antigen and building a 2,4,4'-tribromodiphenyl ether Immunoassay method.

The invention discloses a method of comprehensively use of chloronitrobenzene mixture by fluoro-reaction, comprising steps of: generating a mixture mainly composed of parachloronitrobenzene, o-chloronitrobenzene and m-chloronitrobenzene in process of parachloronitrobenzene, o-chloronitrobenzene by chlorobenzene nitration method; removing low-boiling-point substances by evaporation; then adding anhydrous potassium fluoride and catalyst to the mixture for fluoro-reaction at 150 DEG. C to 250 DEG. C; after reaction, filtering to remove potassium chloride, after rectifying to acquire parachloronitrobenzene, o-chloronitrobenzene, the residual portion via recrystallization acquires m-chloronitrobenzene; the catalyst is quaternary ammonium salt or calixarene; charge rate of chloronitrobenzene mixture and mixture is 1:0.01 to 1. The method of the invention is simple to operate, in scale and changes waste material into things of value, which realizes zero discharge. The method is characterizedin sustainable development, energy saving, consumption reduction and environmentally friendly property.

The invention provides a comprehensive development separation method of m-chloronitrobenzene, p-chloronitrobenzene, and o-chloronitrobenzene mixture. The comprehensive development separation method ofm-chloronitrobenzene, p-chloronitrobenzene, and o-chloronitrobenzene mixture comprises following steps: the m-chloronitrobenzene, p-chloronitrobenzene, and o-chloronitrobenzene mixture, potassium fluoride, and tetrabutylammonium chloride are introduced into a distiller, under vacuum conditions, water vapour in the system is discharged, the temperature is increased to 140 to 145 DEG C, ultrasonicreaction is carried out, the temperature is reduced to 73 to 78 DEG C, water is added, and an oil layer and a water layer are obtained through separation; the oil layer is introduced into an ice waterbath for stirring crystallization, filtering is carried out to obtain filtrate o-fluoronitrobenzene; a crystal product obtained through separation is introduced into a rectifying tower, crystal melting is carried out, tower top temperature is controlled to be 205 to 210 DEG C, tower bottom temperature is controlled to be 235 to 240 DEG C, a non-condensing collector is adopted for rectification, and a p-fluoronitrobenzene crude product and a m-fluoronitrobenzene crude product are obtained; the p-fluoronitrobenzene crude product is heated to 150 to 180 DEG C, is cooled to 50 to 55 DEG C, and iscooled to 25 to 30 DEG C slowly for separation, a filtrate is collected, and purified p-fluoronitrobenzene is obtained; the m-fluoronitrobenzene crude product is cooled to 10 to 15 DEG C, is heated to 30 to 40 DEG C slowly, separation is carried out, and a crystal product is collected to obtain purified m-fluoronitrobenzene.

The present invention belongs to the field of preparation technology of aromatic amine as hole transmission material intermediate. The preparation process of nitro aromatic amine compound includes the following steps: reacting one of phenylamine, diphenylamine and triphenylamine, strong alkali and p-fluoro nitrobenzene or p-chloro nitrobenzene in certain molar proportion in N, N-dimethyl formamide as solvent inside some reactor at 90-130 deg.c for 5-16 hr; filtering in the hot state to eliminate reaction produced impurity; decompression distillation to eliminate DMF and to obtain initial product; and re-crystallization with methanol, ethanol or acetonitrile to obtain the nitro aromatic amine compound. The present invention has the advantages of cheap material, simple post-treatment, high product yield, high product purity and being suitable for industrial production.

The invention discloses a purpurine derivative electrochromic material and a preparation method thereof. The preparation method comprises the steps that 4,4'-dipyridine is adopted as a raw material and undergoes a Menschutkin reaction with 1-chloro-2,4-dinitrobenzene to synthesize a 1,1'-bis(2,4-dinitro)-4,4'-dipyridyl salt; then an N-heterocyclic compound and p-fluoronitrobenzene are subjected toaromatic nucleophilic amination to prepare a 4-nitrocompound, and then the 4-nitrocompound is reduced into a 4-amino compound; finally, the products obtained after the reactions in the two steps undergo a Zincke reaction to obtain a target product. A pyrrole group and carbazole are introduced into a derivative, the electron deficient state of the core group 4,4'-dipyridine of a purpurine compoundis improved, and the electrochromic voltage of the purpurine compound is reduced; moreover,a bipolar electrochromic device can be obtained, a higher contrast ratio is realized, multiple color changesare obtained, and the problem of electrolyte leakage of solution-type electrochromic devices can also be solved.

The invention discloses a preparation method of an alminoprofen intermediate, belongs to the field of organic chemical synthesis, and provides a new technical route for improving the defects of synthetic reaction of ethyl 2-(4-amino-phenyl)propionate: 1) taking p-fluoronitrobenzene and diethyl methylmalonate as raw materials, adding alkali, conducting heating, finishing the reaction, conducting cooling, conducting hydrolyzing with alkali, after the reaction is finished, conducting layering, conducting washing with water, extracting impurities, adjusting the pH value, extracting a product, and conducting concentrating to obtain AMLF02; 2) heating AMLF02 in a solvent to 55-75 DEG C, and dropwise adding thionyl chloride for esterification reaction, conducting cooling, adjusting the pH, directly adding a catalyst for reduction at the temperature of 70-80 DEG C, after the reaction is finished, conducting filtering with the aid of diatomite, neutralizing the filtrate to 7-8, conducting concentrating to remove ethanol, extracting a water phase with methylbenzene, and conducting concentrating to obtain AMLF04. The method has the beneficial effects that the problem of slow filtration is solved, extraction is omitted, time is saved, and cost is saved; direct layering is performed after reaction, the amount of hydrochloric acid is reduced, and the treatment difficulty of three wastes is reduced; and safe hydrazine hydrate replaces active nickel.