43 results about "O-fluoronitrobenzene" patented technology

The invention discloses a catalyst for preparing o-fluoroaniline from o-fluoronitrobenzene by hydrogenation. The catalyst contains an Al2O3 supporter and the following components in percentage by mass: 0.05%-1% of Pt supported on the Al2O3 supporter, 0.05%-3% of metal M1 and 0.01%-3% of metal M2, wherein the metal M1 is Pd, Sn or Zn; the metal M2 is K, Co, Ga, In, Mn, Ag or Ce. Besides, the invention also provides a preparation method of the catalyst. When the catalyst prepared by the preparation method is used for catalyzing o-fluoronitrobenzene hydrogenation, the mole conversion rate of o-fluoronitrobenzene is up to 100%, the mole percentage of a defluorination product is smaller than 0.1%, the amount of o-fluoronitrobenzene treated by the catalyst of unit mass is large, the use amount of the catalyst is small, and the catalyst can be reused after being regenerated.

The invention discloses an industrial preparation method of 1,3-dibromo-4-fluorobenzene. The industrial preparation method of 1,3-dibromo-4-fluorobenzene comprises the steps that o-fluoronitrobenzeneserves as an initial raw material, and 1,3-dibromo-4-fluorobenzene is synthesized through bromine applying, reduction and diazotization-Sandmeyer three step reactions. The obtained 1,3-dibromo-4-fluorobenzene is yellow oily liquid, the purity is 97.5%, the raw material conversion rates of all steps each reach 100%, and the total recovery of the whole process reaches 52.7%.

The invention relates to hydrogenation preparation of 4-aminophenol from nitrobenzene, especially a method for hydrogenation preparation of 4-amino-3-fluorophenol from o-fluoro-nitrobenzene and device therefore. The reaction is carried out in autoclave with acid medium at 50í½300C.,0.1í½10.0MPa, and the stirring rate is 100í½900 r / min, and the catalytically hydrogenated product is separated, distilled, filtered, and dried to prepare the product. O-fluoro nitrobenzene can be converted into 4-amino-3-fluobenzene by said method with conversion approaching 100%. 4-amino-3-fluobenzene is colourless crystallisate with selective around 92% and purity up to 99%. The catalytic process in the invention can be used for heterogeneous catalysis process of hydrogenation preparation of aminophenol from o-fluoro nitrobenzene and its substituted nitrobenzene.

The invention discloses a preparation method of 4-chlorine-3-fluorine benzene ether. The preparation method comprises the following steps: firstly, by taking o-fluoronitrobenzene as a raw material, preparing 4-amino-3-fluorophenol; taking N,N-dimethylformamide as a reaction medium, carrying out acylating chlorination reaction between the 4-amino-3-fluorophenol and an acyl chloride reagent, thus preparing 4-chlorine-3-fluorophenol, mixing sodium phenoxide with a sodium hydroxide aqueous solution, then adding the 4-chlorine-3-fluorophenol, and uniformly stirring and mixing, thus preparing a mixed solution; adding the prepared mixed solution into a reactor, then adding diethyl sulfate, stirring for 3 min, and heating to 80 to 120 DEG C for reaction; at the end of reaction, adjusting the pH ofa reaction system to 2 to 5, allowing the reaction system to stand still for layering, collecting an oil phase, washing the oil phase with the sodium hydroxide aqueous solution, and collecting the oil phase, namely the 4-chlorine-3-fluorine benzene ether. The method disclosed by the invention is easy to operate, low in cost, high in target product purity and high in yield.

The invention discloses a method for preparing o-fluoroaniline by hydrogenating o-fluoronitrobenzene. The method comprises the following steps: 1, filling a fixed bed reactor with a catalyst, introducing air and heating; 2, uniformly mixing o-fluoronitrobenzene steam and preheated hydrogen to obtain mixed gas, introducing the mixed gas into the fixed bed reactor, and performing a catalytic hydrogenation reaction in the presence of the catalyst; and 3, delivering the material subjected to the catalytic hydrogenation reaction into a condenser, condensing the material to convert the o-fluoronitrobenzene steam in the material into a liquid state, and separating the liquid-state o-fluoronitrobenzene in an oil-water separator to obtain oil-state o-fluoroaniline. The o-fluoronitrobenzene is catalytically hydrogenated by adopting the method, the treatment amount is large, the o-fluoronitrobenzene is completely converted, the molar conversion rate of the o-fluoronitrobenzene is 100 percent, and the molar percentage of a defluorinated product is less than 0.1 percent; and the product separating and purifying operation is simple at low energy consumption, and no toxic or harmful ions are doped in the product.

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 invention discloses a catalyst for preparing o-fluoroaniline from o-fluoronitrobenzene by hydrogenation. The catalyst contains an Al2O3 supporter and the following components in percentage by mass: 0.05%-1% of Pt supported on the Al2O3 supporter, 0.05%-3% of metal M1 and 0.01%-3% of metal M2, wherein the metal M1 is Pd, Sn or Zn; the metal M2 is K, Co, Ga, In, Mn, Ag or Ce. Besides, the invention also provides a preparation method of the catalyst. When the catalyst prepared by the preparation method is used for catalyzing o-fluoronitrobenzene hydrogenation, the mole conversion rate of o-fluoronitrobenzene is up to 100%, the mole percentage of a defluorination product is smaller than 0.1%, the amount of o-fluoronitrobenzene treated by the catalyst of unit mass is large, the use amount of the catalyst is small, and the catalyst can be reused after being regenerated.

The invention relates to a synthetic route for preparing olanzapine by using o-fluoro-nitrobenzene as a raw material. In the method, the o-fluoro-nitrobenzene is used as a starting material to prepare the olanzapine by steps of coupling, reduction and ring closing.

The invention belongs to a method for preparing pharmaceutical intermediate, and discloses a method for preparing 3-fluorine-4 morpholinyl phenylamine, comprising the steps: (1) reducing o-fluoro-nitrobenzene to obtain o-fluoroaniline; (2) adding the o-fluoroaniline and deacidifying agent into organic solvent, and slowly adding disubstituted ethyl ether into a reaction system at the temperature of 100-150 DEG C and then stirring at the temperature of 100-200 DEG C to react for preparing o-fluoro-morpholinyl benzene; (3) taking nitric acid with the mass percent of 65-98% as nitrating agent andacetic acid as solvent, and leading the o-fluoro-morpholinyl benzene obtained in the step (2) to have nitration reaction to obtain 3-fluorine-4 morpholinyl nitrobenzene; (4) reducing the 3-fluorine-4morpholinyl nitrobenzene obtained in the step (3) and obtaining the 3-fluorine-4 morpholinyl phenylamine. As the method takes the o-fluoro-nitrobenzene as initial reactant, the price of the raw materials is low, and the production cost can be reduced. Meanwhile, no waste water containing fluorine is generated in the preparation process of the method, so that the method has little environmental pollution and is environment-friendly.

The invention discloses a synthetic method for 3-amino-4-fluorophenylboronic acid. The method includes the steps of conducting bromination on o-fluoronitrobenzene, conducting reduction to generate 5-bromo-2-fluoroanil, making 5-bromo-2-fluoroanil and tetrahydroxydiboron react in a coupled mode to generate the product, namely, 3-amino-4-fluorophenylboronic acid. According to the method, raw materials can be easily obtained, and operation is easy and convenient. The method is an appropriate route for preparing 3-amino-4-fluorophenylboronic acid.