528 results about "Friedel–Crafts reaction" patented technology

The invention relates to a process for preparing 4,4'-dichlorodiphenylsulfone, in particular to a process for preparing 4,4'-dichlorodiphenylsulfone employing a sulfoxide oxidation method. The process comprises the following steps: carrying out friedel-crafts reaction with chlorobenzene and thionyl chloride under the action of a catalyst to obtain the 4,4'-dichlorodiphenylsulfone; dissolving the obtained 4,4'-dichlorodiphenylsulfone with a solvent; adding hydrogen peroxide and carrying out oxidation reaction to obtain a 4,4'-dichlorodiphenylsulfone crude product; carrying out secondary oxidation refining on the obtained 4,4'-dichlorodiphenylsulfone crude product; and finally preparing high-purity 4,4'-dichlorodiphenylsulfone. The purity of the 4,4'-dichlorodiphenylsulfone purified by the refining process is greater than 99.5%; the refining yield is greater than 98.5%; and the process completely meets the synthesis requirements of high-performance polymers.

The invention discloses a preparation method of improved 4,4-dichlorodiphenylsulfone. The method comprises steps that: (1) Al2Cl3 is adopted as a catalyst; chlorobenzene, thionyl chloride are adopted as reaction materials; the materials are subject to a Friedel-Crafts reaction; a mother liquor obtained after the reaction is hydrolyzed; the hydrolyzed mother liquor is refluxed for 45 to 60min under a temperature of 95 to 100 DEG C; after refluxing, the mother liquor is cooled to below 20 DEG C, such that the liquor is divided into an organic phase and a water phase; the organic phase is processed through reduced-pressure distillation and centrifugal washing until the organic phase turns neutral, and the organic phase is preserved as a product M for later use, wherein a main component in the product M is 4,4-dichlorodiphenylsulfone; (2) the product M and an oxidizing agent of hydrogen peroxide are adopted as raw materials, and 1,2-dichloropropane is adopted as an organic solvent; an oxidizing reaction is carried out upon the main component 4,4-dichlorodiphenylsulfone in the product M under the effect of a composite catalyst, such that a 4,4-dichlorodiphenylsulfone crude product is synthesized, wherein the composite catalyst is phosphotungstic acid or silicotungstic acid loaded on active carbon. Therefore, the method provided by the invention has advantages of high yield and good product quality. With the method, wastewater can be circulated and reused.

The invention discloses a new preparation method of 4,4-dichlorodiphenyl sulfone. The method comprises the following steps: 1) through using AlCl3 as a catalyst, and chlorobenzene and thionyl chloride as reaction raw materials, performing a Friedel-Crafts reaction at 25-35 DEG C, then hydrolyzing the mother liquor obtained through the Friedel-Crafts reaction, refluxing at 95-100 DEG C for 45-60 minutes, cooling the obtained mother liquor to less than 20 DEG C after refluxing to obtain an organic phase and an aqueous phase; 2) performing reduced pressure distillation on the organic phase, centrifuging, washing the obtained product to be neutral and be used as a product A for later use, wherein the main component of the product A is 4,4-dichlorodiphenyl sulfoxide; and 3) through using the product A and the oxidant hydrogen peroxide as raw materials and acetic acid as satalytic solvent, carrying out an oxidation reaction on the main component 4,4-dichlorodiphenyl sulfoxide of the product A to obtain crude 4,4-dichlorodiphenyl sulfone. Therefore, the existing synthesis method of 4,4-dichlorodiphenyl sulfone is changed, the production cost of 4,4-dichlorodiphenyl sulfone is low, the product quality is good and the reaction time is short.

A novel acidic ionic liquid which is useful as a catalyst for alkylation, nitration, Beckmann rearrangement, etc. and is stable to air and water. It is an ionic liquid represented by the following formula (1): (1) wherein X represents halogeno or hydroxy; Y<-> represents CF3SO3<->, BF4<->, PF6<->, CH3COO<->, CF3COO<->, (CF3SO2)2N<->, (CF3SO2)3C<->, F<->, Cl<->, Br<->, or I<->; n is an integer of 2 to 16; and R represents methyl, allyl, or vinyl. This ionic liquid not only functions as a BrDnsted acid or a Lewis acid but is a liquid insoluble in many organic solvents. The liquid is hence useful as a catalyst or solvent for Friedel-Crafts reaction, nitration, and Beckmann rearrangement. It can be easily separated from the reaction mixture and reused.

The invention discloses a method for preparing functionalized graphene and a composite material of the functionalized graphene. The method for preparing the functionalized graphene comprises the following steps of: performing Friedel-Crafts reaction on natural graphite which is taken as a raw material to obtain modified graphite, extracting, purifying, and uniformly dispersing in an organic solvent with ultrasonic to form stable graphene suspension liquid. The method for preparing the composite material comprises the following steps of: adding epoxy resin into the graphene suspension liquid, stirring for dissolving, uniformly mixing with ultrasonic, distilling under reduced pressure to remove the organic solvent to obtain a graphene/epoxy resin composite; and adding an epoxy resin curing agent, an accelerant and micrometer silver sheets sequentially, and heating for curing to obtain the composite material of a graphene polymer, namely a graphene/epoxy resin conducting composite material. The edge functionalized graphene has a high interaction between functional groups at the edge and a polymer matrix, so that the dispersion of the graphene in the polymer matrix can be promoted, the agglomeration degree can be reduced, and the interface performance of the composite material can be enhanced.

The invention provides a method to prepare a compound method, including the steps: ethylbenzene and capryl chloride make Friedel-Crafts reaction to generate p-capryl chloroethylbenzene; convert capryl chloroethylbenzene under the action of sodium iodide into p-capryl iodoethylbenzene; p-capryl iodoethylbenzene and acetylamino diethyl malonate condense under the action of alkali to generate 2-(p-capryl phenethyl)-2-acetylamino diethyl malonate; or p-capryl iodoethylbenzene makes elimination reaction under the action of alkali to generate p-capryl styrene, which together with acetylamino diethyl malonate condenses under the action of alkali into 2-(p-capryl phenethyl)-2- acetylamino diethyl malonate; a compound is reduced into 2-[4-(1-hydroxyoctyl) phenethyl-]2- acetylamino propylene alcohol; the other coumpound makes hydrogenolysis to obtain 2-(p-octyl phenethyl)-acetylamino propylene alcohol; make alkali hydrolyzation and then acidifies them into salt, so as to obtain it. It also provides a method to prepare intermediate in the above preparing course.

The invention discloses a preparation method, a material and an application of a porous polymer. The preparation method comprises the following steps: (1) evenly dispersing the raw material (aromatic compounds, mixtures of the aromatic compounds, polymers of the aromatic compounds and/or mixtures of the polymers) into a crosslinking agent and solvent, so as to obtain a raw material mixed solution, wherein the crosslinking agent solvent is one or more of alkane dihalides; (2) adding a catalyst, carrying out Friedel-Craft reaction, and carrying out super-crosslinking, so as to obtain a crude product; and (3) washing and extracting a filter cake which is obtained after the coarse product is filtered, removing a catalyst, and drying, so as to obtain a porous polymer. The preparation method disclosed by the invention is simple in process, uses easily available raw materials, the prepared porous polymer is adjustable in pore size and specific surface area, has low cost and good adaptability, and can be used as a catalyst carrier, a separation membrane, a gas storage material or an ion adsorbing material, especially, can be used as materials for storing hydrogen and capturing carbon dioxide or methane storage materials.

The invention provides a new method for preparing dexmedetomidine hydrochloride. According to the method, Lewis acid is used as a catalyst, and racemized medetomidine is prepared by a Friedel-Crafts reaction; and the racemized medetomidine is resolved by (+)-di-p-toluoyl-tartaric acid [(+)-DDTA] to obtain dexmedetomidine. The dexmedetomidine is salified in hydrochloric acid to obtain dexmedetomidine hydrochloride.

The invention discloses a bis (imino) pyridine iron olefin polymerization catalyst and a preparation method and application thereof. The catalyst is a novel bis(imino)pyridine iron complex with the asymmetric substitution of position 2 and 6 of an aromatic ring; and the structural formula of the catalyst is shown in formula (I), wherein X is halogen, R1 is alkyl, and R2 is the alkyl or oxyl. The catalyst can be obtained through a Friedel-Crafts reaction, a ketoamine condensation reaction and a coordination reaction. The preparation method is simple, and raw materials are cheap. The catalyst can catalyze the polymerization of ethylene under the activation of MAO to prepare polyethylene with high molecular weight and wide distribution.

The invention discloses a nitrogen and sulfur co-doped carbon-loaded non-noble metal type oxygen reduction catalyst and a preparation method thereof and discloses a M-N-S-C oxygen reduction catalyst and a preparation method thereof. The raw materials of the catalyst comprise copolymer P (TPT+Tp) of tripyrrole-[1,3,5]-triazine (TPT) and thiophene (Tp) and non-noble metal salt. The preparation method of the catalyst includes the following steps that firstly, a Friedel-Crafts reaction is adopted for synthesizing the copolymer P (TPT+Tp) of the tripyrrole-[1,3,5]-triazine (TPT) and the thiophene (Tp); secondly, the P (TPT+Tp) and the non-noble metal salt are added into ethanol, mixtures are placed in an ultrasonic dispersing instrument, a whole system is evenly dispersed due to ultrasound, and then the ethanol is dried by distillation and placed in a vacuum drying box to be dried for 4 h at the temperature of 80 DEG C; thirdly, thermal treatment is performed for the first time and nitrogen doped materials are obtained; fourthly, the nitrogen doped materials are completely washed through dilute acid; fifthly, thermal treatment is performed for the second time, and then the M-N-C oxygen reduction catalyst can be obtained.

The invention discloses an M-N-C oxygen reduction catalyst and a preparation method thereof, wherein the raw materials of the catalyst comprise a copolymer (P(TPT+Py)) of tripyrrole-[1,3,5]-triazine (TPT) and pyrrole (Py) and a non-noble metal salt. The preparation method comprises: (1) using a Friedel-Crafts reaction to synthesize a copolymer (P(TPT+Py)) of tripyrrole-[1,3,5]-triazine (TPT) and pyrrole (Py); (2) adding (P(TPT+Py)) and a non-noble metal salt to ethanol, placing into an ultrasonic dispersion device, carrying out an ultrasonic treatment to make the whole system be uniformly dispersed, evaporating the ethanol, placing into a vacuum oven, and drying for 4 h at a temperature of 80 DEG C; (3) carrying out a first heat treatment to obtain a nitrogen-doped carbon material; (4) completely washing the obtained nitrogen-doped carbon material with a diluted acid; and (5) carrying out a second heat treatment so as to obtain the M-N-C oxygen reduction catalyst.

The invention relates to a fluorenyl organic framework material, a preparation and application method thereof. A material which is provided with a framework structure shaped as a Chinese character ri and constructed by the method disclosed by the invention is taken as a new generation organic semiconductor to be applied to an organic electronic device. The structure of the material is shown in the specification. The material has the characteristics that (1) monomers are synthesized via a Grignard reaction and a Friedel-Crafts reaction, the raw material is inexpensive and the synthesis method is simple; (2) the material has high heat stability and glass transition temperature; (3) the material is good in flexibility and high in solubility; and (4) due to the accumulation effect of diaryl fluorine, the material is good in electrooptic activity. The fluorenyl organic framework material can be applied to the organic electronic field of film devices such as organic light emitting display, organic light storage, organic photovoltaic cells, organic field effect transistors and organic laser, and the like. Electroluminescent devices prepared by using the material disclosed by the invention show satisfactory results in luminance, luminous efficiency and voltage resistance stability.

The invention relates to the field of medicinal chemistry, and discloses a method for preparing mangiferin aglycone. The method comprises that: step 1, 2-halogenate-4,5-dimethoxy benzoic acid and 1,3,5-trimethoxy benzene are subjected to Friedel-Crafts reaction, so a compound which has a structure in a formula IV is generated; step 2, the compound in the formula IV is selectively demethylated, and a compound which has the structure in the formula V is generated; step 3, the compound in the formula V is cyclized, and a compound which has the structure in the formula VI is generated; and step 4, the compound in the formula VI is completely demethylated, and mangiferin aglycone is generated. The method for preparing mangiferin aglycone improves the synthetic yield of the mangiferin aglycone, has the characteristics of cheap and easily-obtained raw materials, less synthetic steps, convenience in operation, easiness in control and high product purity, and can be widely applied in industrial production.

The invention offers 2-amphi capryl phenethyl-2-amino group propylene glycol hydrochloride preparation method. It includes the following steps: doing Friedel-Crafts reaction for styrene and capryl chloride to produce amphi capryl styrene; doing Michael addition reaction with kharophen diethyl malonate under alkali action to produce 2-amphi capryl phenethyl-2-kharophen diethyl malonate; reacting with triethyl silane to produce 2-amphi capryl phenethyl-2-kharophen diethyl malonate; reducing and hydrolyzing to produce 2-amphi capryl phenethyl-2-amino group propylene glycol; acidifying with hydrochloric acid to produce salt. It has the advantages of simple line, low cost, short period, little pollution, and high yield. It also offers the intermediate compound preparation method.

The invention relates to a preparation method of 2-hydroxyl-1-{4-(2-hydroxyethyl) phenyl}-2-methyl-1-acetone, which comprises the following steps that: ethylene glycol phenyl ether acetate serves as the raw material and carries out friedel-crafts reaction with isobutyl chloride with the molar ratio of 1 to 1.2 times of equivalent under the catalysis of lewis acid, the reaction temperature is -5 to 5DEG C, and the reaction time is 3 to 6h; bromination is carried out under the catalysis of N, N-dimethylformamide or iodine; at room temperature, phase transfer catalyst is used for carrying out catalysis and hydrolysis to a brominated product; and finally the product is prepared through purification and crystallization. The preparation method of 2-hydroxyl-1-{4-(2-hydroxyethyl) phenyl}-2-methyl-1-acetone adopts dichloromethane or dichloroethane as the solvent during the bromination process, does not use acetic acid any more, carries out reaction under the catalysis of DMF or I2, so that the reaction time is greatly shortened. The phase transfer catalyst is introduced during the hydrolysis process, so that the intermediate brominated product directly has reaction with alkali in water, thereby preventing using a large amount of ethanol as the solvent, simplifying the process, reducing the production cost and improving the yield.

The invention discloses a compound containing a tetraphenyl ethylene unit, a preparation method and applications thereof. The preparation method comprises following steps: taking aniline derivatives as the initial reactants, obtaining the key intermediate diphenylketone through the Friedel-Crafts reactions catalyzed by copper, then obtaining tetraphenyl ethylene mono bromine derivatives and tetraphenyl ethylene mono boric acid ester derivatives through further reactions, and finally obtaining the object compound through the Suzuki coupling reactions. The compound containing a tetraphenyl ethylene unit has a good thermal stability and an excellent aggregation-induced emission property. The fluorescence quantum yield of the solid compound is high, and the fluorescent is blue light emission or dark blue light emission, so the compound can be used as the material of the luminous layers of organic light emitting diodes, which give off blue lights or dark blue lights. The preparation method has the advantages of mild reaction conditions and high yield.

The invention relates to a preparation method of 2-(5-bromo-2-methylbenzyl)-5-(4-fluorophenyl)thiophene, which comprises the following steps: carrying out coupling reaction on 2-bromothiophene and p-bromofluorobenzene to obtain 2-(4-fluorophenyl)thiophene; carrying out Friedel-Craft reaction on the 2-(4-fluorophenyl)thiophene and 2-methyl-5-bromobenzoic acid to obtain 5-bromo-2-methylphenyl-2-(4-fluorophenyl)thienyl ketone; and finally, carrying out reduction reaction on the 5-bromo-2-methylphenyl-2-(4-fluorophenyl)thienyl ketone to obtain the 2-(5-bromo-2-methylbenzyl)-5-(4-fluorophenyl)thiophene. By using the cheap and accessible p-bromofluorobenzene and 2-methyl-5-bromobenzoic acid as the raw materials for synthesizing the canagliflozin intermediate, the product is easy for purification, and the method is simple to operate and has the advantages of low cost and environment friendliness.

The invention provides a preparation method of vilazodone, which comprises the following steps: reacting 5-cyanoindole, which is used as the initial raw material, with substituted phenylsulfonyl chloride under alkaline conditions, carrying out Friedel-Crafts reaction under the catalytic action of Lewis acid, reducing the product, and carrying out substitution reaction with 5-(1-piperazino)-benzofuryl-2-formamide to obtain the vilazodone. The invention also provides three intermediate compounds related to the vilazodone preparation method. The preparation method provided by the invention has the advantages of low cost, high yield and simple after-treatment, and is easy to operate and convenient for industrial production; and all the reagents are conventional reagents.

The invention relates to a preparation method of ultra-high crosslinking type adsorptive resin modified by N-methyl acetamido. Lewis acid is added into a chlorine ball swollen in a solvent to be as a catalyst, and Friedel-Crafts reaction is carried out at 80 to 100 DEG C so as to obtain the ultra-high crosslinking type adsorptive resin; and the obtained resin is further aminated and acetylated soas to prepare the ultra-high crosslinking type adsorptive resin modified by the N-methyl acetamido. According to the preparation method of the ultra-high crosslinking type adsorptive resin modified by the N-methyl acetamido, the surface of the ultra-high crosslinking type adsorptive resin is loaded with the N-methyl acetamido, which can obviously enhance the adsorption capacity of the resin to weak polar and polar substances (such as phenol and salicylic acid). The ultra-high crosslinking type adsorptive resin modified by the N-methyl acetamido has an extensive application prospect in the fields of the treatment, the recycle and the like of phenols and organic acid wastewater.

The invention discloses a preparation method and an application of polar group-modified pendent double bond post-crosslinked polydivinylbenzene resin. The preparation method comprises: firstly performing a polymerization reaction of divinylbenzene monomers, polar monomers, and a pore forming agent to obtain a polar group-modified pendent double bond post-crosslinked polydivinylbenzene resin precursor; performing further crosslinking through a Friedel-Crafts reaction to obtain the polar group-modified pendent double bond post-crosslinked polydivinylbenzene resin. The preparation method is simple, and low in cost, and the prepared post-crosslinked resin has a high specific surface area and a special pore structure; the post-crosslinked resin can be used for adsorbing and removing organic matter in waste water, has the effect of selective adsorption, and especially has obvious selective adsorption effect on Congo red and/or rhodamine B.