241 results about "Bromobenzene" patented technology

The invention discloses water-based formaldehyde-free woodworking glue and a preparation method thereof, and relates to the technical field of woodworking glue. When the water-based formaldehyde-free woodworking glue is prepared, firstly, n-butyllithium is used as an initiator to initiate cyclosiloxane and an acrylate monomer to be polymerized, then dimethyl chlorosilane is used for blocking to obtain pre-modified polyacrylate, and the pre-modified polyacrylate is used for preparing the water-based formaldehyde-free woodworking glue. Reacting the pre-modified polyacrylate with vinyl diphenylphosphine, and then reacting with 3-(4-bromophenyl)-1-propylene to obtain modified polyacrylate; secondly, reacting the 4-(trimethoxysilyl) butyraldehyde modified silicon dioxide with chitosan, and then reacting with mercaptoacetic acid to obtain modified silicon dioxide; finally, mixing the modified polyacrylate, the modified silicon dioxide, an emulsifier, a defoaming agent, pure water and a photoinitiator to obtain the water-based formaldehyde-free woodworking glue. The water-based formaldehyde-free woodworking glue prepared by the invention has flame retardance and antibacterial property.

The invention discloses an extraction agent for extracting lithium from lithium precipitation mother liquor and an extraction method. The lithium extraction extracting agent comprises a solute and an organic solvent, the solute comprises at least one of 2, 3, 7, 8-tetraaminophenazine-1, 4, 6, 9-tetraketone and terpyridyl, and the organic solvent comprises at least one of dichloromethane, trichloromethane, carbon tetrachloride, bromobenzene and carbon disulfide. The lithium extraction extractant can be used for extracting lithium in the lithium precipitation mother liquor in a wide pH range, lithium ions enter the lithium extraction extractant and then are rapidly complexed with solutes in the lithium extraction extractant to form a solid phase, the extracted mixed liquor A only needs to be subjected to standing and phase splitting, lithium exists in a lithium-containing solid complex of a lower-layer oil phase, and the lithium precipitation mother liquor in the lower-layer oil phase does not exist in the lithium-containing solid complex. The lithium-containing solid complex can be obtained by filtering the lower-layer oil phase, the residual amount of sodium in the lithium-containing solid complex is small, in addition, the extraction method can omit the working sections of rear-end washing, reverse extraction and the like of a traditional extraction technology, the extraction technological process is shortened to a large extent, and the production cost is saved.

The invention discloses a water body heavy metal ion pollution treatment adsorption filtering membrane and a preparation method thereof, and relates to the technical field of water treatment. When the water body heavy metal ion pollution treatment adsorption filtering membrane is prepared, graphene oxide sequentially reacts with 3-diethylaminopropylamine, tetrabromophenyl porphyrin and N, N-diethyl allylamine, and functionalized graphene oxide is prepared; the preparation method comprises the following steps: reacting cellulose with 4 '-bromo-2, 2': 6 ', 2' '-terpyridyl and maleic anhydride in sequence to prepare modified cellulose; the preparation method comprises the following steps: reacting sodium alginate with propylene oxide to prepare modified sodium alginate; the modified sodium alginate, the modified cellulose, the functionalized graphene oxide, trans, trans-1, 3-butadiene-1, 4-dicarboxylic acid and a photoinitiator are subjected to a reaction, a membrane is prepared, and the water body heavy metal ion pollution treatment adsorption filtering membrane is prepared. The water body heavy metal ion pollution treatment adsorption filtering membrane prepared by the invention has good antibacterial and photocatalytic organic matter degradation capabilities.

The invention discloses an application of 3, 4, 5-trifluorobromobenzene in an electric storage polymer coating, and the electric storage polymer coating is prepared from hyperbranched polyimide based on 3, 4, 5-trifluorophenyl through a spin coating method. The coating is high in solubility, good in processability and low in water absorption; the hyperbranched polyimide is formed by polymerizing a diamine compound containing 3, 4, 5-trifluorophenyl and polybasic acid anhydride, the hyperbranched polyimide has a triphenylamine structure and trifluorophenyl, tight packing of molecular chains can be improved under the combined action of torsional motion of the triphenylamine structure and the trifluorophenyl, and meanwhile, the electronegativity of F atoms is high, so that the polarity of molecules can be increased, and the hydrophobic performance can be improved.

The invention provides continuous production equipment and a production method of 3, 4, 5-trifluorobromobenzene, the continuous production equipment comprises a continuous feeding device, the continuous feeding device is used for continuously supplying a first reaction raw material and a second reaction raw material, the first reaction raw material is o-dichlorobenzene, and the second reaction raw material is chlorosulfonic acid; an inlet of the continuous sulfonation reaction tank is communicated with an outlet of the continuous feeding device, and the continuous sulfonation reaction tank is used for providing a reaction place for a continuous sulfonation reaction of the first reaction raw material and the second reaction raw material so as to obtain a continuous sulfonation product; an inlet of the continuous post-treatment device is communicated with an outlet of the continuous sulfonation reaction tank, so that continuous post-treatment is performed on the continuous sulfonation product, 3, 4, 5-trifluorobromobenzene is obtained, and the problems caused by batch reaction in the prior art are solved.

The invention discloses an active oxygen activated near-infrared region photo-thermal reagent and a preparation method and application thereof.The near-infrared region photo-thermal reagent with active oxygen response is constructed by means of etherification reaction of phenolic hydroxyl functionalized aza-BODIPY dye and p-bromophenylboronic acid pinacol ester and further prepared into nanoparticles, and the near-infrared region photo-thermal reagent with the active oxygen response function is prepared into the active oxygen activated near-infrared region photo-thermal reagent. After the nano particle reacts with active oxygen, the photo-thermal efficiency of the nano particle is remarkably improved under 808nm laser illumination, and the nano particle has an excellent photo-thermal imaging effect and a photo-thermal treatment function.

The invention provides a cationic conjugated polymer as well as a preparation method and application thereof. The structural formula of the cationic conjugated polymer is shown in the specification. The preparation method comprises the following steps: reacting tris (4-bromophenyl) amine and N, N-dimethyl-4-(4, 4, 5, 5-tetramethyl-1, 3, 2-dioxaborolane-2-yl) aniline in an organic solvent under the action of a catalyst and an initiator to obtain a first intermediate; the cationic conjugated polymer is prepared from the first intermediate, the second intermediate and the third intermediate under the action of a catalyst and an initiator. The cationic conjugated polymer shows good photo-thermal and photodynamic performance under the irradiation of near-infrared light with the wavelength of 980 nm, so that the effect of inhibiting the growth of bacteria is realized. # imgabs0 #

The invention relates to the technical field of organic synthesis, and provides a preparation method of alkylpyran-3, 5-difluorobenzene, which comprises the following steps: S1, adding a Grignard reagent into an alkylpyrone solution, reacting for the first time, quenching for the first time, separating liquid to obtain an organic phase, adding acidic resin into the organic phase, refluxing, and filtering to obtain filtrate containing alkylpyranene chlorobenzene, sequentially adding tetramethyldisiloxane and methanesulfonic acid into the filtrate containing the alkylpyran chlorobenzene, and carrying out a second reaction to obtain alkylpyran chlorobenzene; s2, adding alkylpyran chlorobenzene, 3, 5-difluorophenylboronic acid and an acid-binding agent into the solvent, stirring, adding a catalyst, and carrying out a third reaction to obtain alkylpyran 3, 5-difluorobenzene; the Grignard reagent is prepared from magnesium chips and p-chlorobromobenzene. According to the technical scheme, the problems of high preparation cost and low purity and yield of the alkylpyran 3, 5-difluorobenzene in the prior art are solved.

The invention discloses a triphenylamine supramolecular polymer capable of adjusting circularly polarized light as well as a preparation method and application thereof. The polymer is formed by co-assembling a triphenylamine donor and a naphthalene monoamide acceptor through intermolecular non-covalent acting force; the preparation method of the triphenylamine donor comprises the following steps: S1, adding methyl gallate and bromododecane into DMF (Dimethyl Formamide), and reacting to obtain a compound A; s2, adding the compound A and sodium hydroxide into ethanol to react to obtain a compound B; s3, adding the compound B, 1-(4-bromophenyl) ethylamine, 1-ethyl-(3-dimethylaminopropyl) carbodiimide and 4-dimethylaminopyridine into dichloromethane, and carrying out a reaction so as to obtain a compound C; s4, adding the compound C, Pd (PPh3) 2Cl2, CuI and trimethylsilylacetylene into triethylamine in an inert atmosphere, and reacting to obtain a compound D; and S5, adding the compound D, Pd (PPh3) 2Cl2, CuI and tris (4-iodophenyl) amine into triethylamine in an inert atmosphere, and reacting to obtain the triphenylamine donor. The invention develops a CPL material with a wide-range tunable characteristic.

The invention belongs to the technical field of solar cells, and particularly relates to a triphenylamine-containing conjugated polymer hole transport layer material and a preparation method thereof. The preparation method of the triphenylamine conjugated polymer comprises the following steps: reacting aniline with bromobenzene under the action of a catalyst to generate a compound 1; reacting the compound 1 with NBS (N-bromosuccinimide), and performing bromination reaction to obtain a compound 2; reacting the compound 2 under the action of bis-pinacol diboron, potassium acetate and a catalyst to obtain a compound 3; the method comprises the following steps: dissolving a monomer 1, a monomer 2 and a catalyst in an organic solvent, and carrying out polymerization reaction under the protection of nitrogen to obtain the triphenylamine conjugated polymer. The synthetic route is simple, the yield is high, conditions are easy to realize, and the hole transport layer material prepared from the conjugated polymer of triphenylamine is high in transport efficiency and can be popularized in a large range.

The invention relates to a synthesis process of an omarigliflozin intermediate, and belongs to the technical field of drug synthesis, one-step efficient conversion is adopted in the process of synthesizing the omarigliflozin intermediate, p-bromophenylhydrazine hydrochloride is used as a starting raw material, and a target product is obtained through indole cyclization, alkali precipitation and acidification crystallization. Toluene plays a role in cyclization and dehydration in a high-temperature reflux process, in a purification process of alkali precipitation and acidification crystallization, a sodium hydroxide aqueous solution is utilized to hydrolyze and convert a product into water-soluble sodium salt, the water-soluble sodium salt enters a water phase, a toluene layer containing a large amount of organic impurities and the water phase are layered in a standing and layering process, and the organic impurities in the toluene layer are removed; the preparation method comprises the following steps of: preparing a sodium salt, acidifying in a water phase by using hydrochloric acid, changing the sodium salt form of the product into an acid form, and crystallizing from the water phase, which is equivalent to recrystallization purification, so that the prepared product has higher purity, the purity is stabilized at 98% or above, and the purity of the product can meet the quality standard of medical intermediates.

The application provides an ester-based electrolyte containing a bromobenzene additive for a sodium metal battery and a sodium metal battery, the ester-based electrolyte comprising a bromobenzene additive, an ester-based solvent and a sodium salt; the bromobenzene additive accounts for 1-10 vol% of the ester-based electrolyte. The electrolyte realizes spherical growth of sodium and reduces the formation of 'dead sodium'; the amount of the electrolyte additive is small, the effect of improving the sodium metal deposition morphology and cycle stability is remarkable, and the electrolyte has great industrialization potential.

The invention relates to an organic crystalline piezoelectric material based on chiral 4-bromophenylethylamine hydrochloride, which is synthesized by using hydrochloric acid as an anion and protonated (R / S)-4-bromophenylethylamine as a cation according to the stoichiometric ratio of (R / S)-4-bromophenylethylamine to hydrochloric acid of 1: 1. The invention provides an organic crystalline piezoelectric material based on chiral 4-bromophenylethylamine hydrochloride and a preparation method, and provides a two-dimensional hydrogen bond network construction strategy based on protonated chiral amine: protonated (R / S)-4-bromophenylethylamine cations are used as structural elements, chloride ions are used as charge balance bodies, and the chiral 4-bromophenylethylamine hydrochloride is prepared by precisely regulating the interaction of intermolecular hydrogen bonds. Constructing a two-dimensional hydrogen bond network with high orientation; by enhancing ordered arrangement of molecular dipoles and optimizing a lattice strain-polarization response collaborative mode, breakthrough improvement of piezoelectric performance is successfully realized, and a new normal form is provided for developing high-performance organic piezoelectric materials.

Belonging to the technical field of fine chemical product separation and purification, the invention discloses a beta-bromophenylethane rectification purification process, which comprises the steps of system negative pressure pretreatment, falling film evaporation directional separation, structured packing layer gas-liquid mass transfer, precise reflux ratio regulation and control, segmented collection (front fraction-qualified product), and residual liquid treatment and system circulation. According to the process, the negative pressure of a system is stabilized at 800-1200 Pa, the material temperature of a falling film evaporation discharging end is controlled at 125-135 DEG C, the feeding flow is stabilized at 1.8-2.2 m / h, the reflux ratio is regulated and controlled at 0.8: 1-1.2: 1, and the process realizes efficient purification of beta-bromopheny ethane through precise negative pressure control, synergistic linkage of falling film evaporation and a rectifying tower, segmented material collection and a circular treatment mechanism, so that the process is suitable for industrial production of beta-bromopheny ethane. According to the method, the purity of beta-bromopheny ethane can stably reach 99.5% or above, the material recovery rate is increased to 92% or above, energy consumption is reduced by 15-20% compared with that of a traditional process, material thermal decomposition loss is avoided, and the method is suitable for industrial large-scale production.

The invention discloses a ferrocene-based D-A type multi-system conjugated small molecule synthesis method, which comprises: carrying out a heating reaction in an organic solvent by using a ferrocenyl compound and a bromophenyl compound as raw materials and using a palladium complex as a catalyst, and after the reaction is completed, carrying out extraction, column chromatography and recrystallization to prepare an intermediate; the obtained intermediate and a 4-pyridine boric acid compound are used as raw materials, a palladium complex is used as a catalyst, a heating reaction is conducted in an organic solvent, and after the reaction is finished, cooling, extraction, column chromatography and recrystallization are conducted to prepare the D-A type multi-system conjugated small molecules. The invention also discloses a memory device with a sandwich structure and application of the memory device to ultra-high density information storage. The small molecular material prepared by the invention not only can realize ternary information storage performance, but also greatly improves the stability of the device through stable redox cycle of the ferrocene group, and realizes long-time stable ultrahigh-density information storage.

The invention relates to a one-pot synthesis method of a fluxapyroxad intermediate 3 ', 4', 5 '-trifluoro-2-nitrobiphenyl, and belongs to the technical field of organic synthesis.The method comprises the following steps that 1, under nitrogen protection, magnesium chips, a catalyst and a solvent are added into a reaction flask, then a mixed solution of 3, 4, 5-trifluorobromobenzene, o-chloronitrobenzene and boric acid ester is dropwise added, a reaction is conducted for 1-2 h, and a reaction solution is obtained; after dropwise adding, carrying out heat-preservation reaction; 2, after the reaction is finished, 10% diluted hydrochloric acid is added for acidification and water washing, after phase splitting, an obtained organic phase is subjected to vacuum concentration, and 3 ', 4', 5 '-trifluoro-2-nitrobiphenyl is obtained. Compared with a traditional synthesis method of the fluxapyroxad intermediate, the synthesis method of the fluxapyroxad intermediate has the advantages that 3, 4, 5-trifluorophenylboronic acid does not need to be prepared firstly, 3, 4, 5-trifluorobromobenzene and o-chloronitrobenzene are directly used as raw materials, the one-pot synthesis method is short in reaction route and high in raw material utilization rate, and the raw material cost can be greatly reduced.

The invention relates to the field of chemistry, and discloses a method for continuously synthesizing 3, 5-dihalogen bromobenzene by using a continuous flow reactor, which is used for continuously synthesizing 3, 5-dihalogen bromobenzene by using the continuous flow reactor for the first time, changes a traditional kettle process into a continuous process, solves a series of problems of long reaction time, high safety risk and the like of batch-type reaction, and improves the yield of 3, 5-dihalogen bromobenzene. According to the present invention, the reaction conditions are mild, the reaction parameters of the 3, 5-dihalogen bromobenzene are optimized, the use of the expensive raw material or solvent is avoided, the raw material is simple and easily available, and the method has advantages of low production cost, simple operation, environmental protection, mild reaction, short reaction time, safe reaction safety compared with the conventional method, high conversion rate, less impurity, simple post-treatment, and industrial production benefiting, and can be used for industrial production of 3, 5-dihalogen bromobenzene. Compared with the prior art, obvious technical progress is achieved.

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of 2-(4-bromophenyl) norcamphane. According to the invention, the proper catalyst is selected to promote the norbornene to be directly added with the bromobenzene Grignard reagent, so that the use of expensive raw materials is avoided, the reaction difficulty is reduced, and the reaction can be smoothly carried out, thereby effectively improving the reaction yield of the 2-phenyl norcamphane. According to the bromination reaction of the 2-phenyl norcamphane, proper catalysts and reaction conditions are selected, and the selectivity of para-products is improved, so that the product yield of the 2-(4-bromophenyl) norcamphane is improved.

The invention belongs to the technical field of pesticide chemistry, and particularly relates to an application of a substituted phenylhydrazine copper salt complex as an agricultural fungicide, the structural general formula of the substituted phenylhydrazine copper salt complex is [Cu (ArNHNH2) 2] Xn, Ar is selected from 3-chlorphenyl-, 2, 4-dichlorophenyl-, 2, 4-dichlorophenyl-, 2, 4-dichlorophenyl-, 2, 4-dichlorophenyl-, 2, 4-dichlorophenyl-, 2, 4-dichlorophenyl-, 2, 4-dichlorophenyl-, 2, 4-dichlorophenyl-, 2, 4-dichlorophenyl-, the compound is prepared from 2, 6-dichlorophenyl, p-trichloromethoxyphenyl, 4-trifluoromethylphenyl, 4-trifluoromethoxyphenyl, 4-bromophenyl, 4-nitrophenyl, 4-cyanophenyl and 4-carboxyphenyl, and the compound is prepared from 2, 6-dichlorophenyl, p-trichloromethoxyphenyl, 4-trifluoromethylphenyl, 4-trifluoromethoxyphenyl, 4-bromophenyl, 4-nitrophenyl, 4-cyanophenyl and 4-carboxyphenyl. X is selected from SO4 <->, Cl <-> and NO3 <->; n is equal to 1-2. The substituted phenylhydrazine copper salt complex disclosed by the invention has remarkable inhibitory activity on plant pathogenic bacteria, has very high inhibition rate on three plant pathogenic fungi, namely fusarium graminearum, rhizoctonia solani and sclerotium rolfsii, can be used as a safe and efficient novel bactericide, and is applied to prevention and treatment of various crop diseases.

The invention relates to the technical field of intermediate synthesis, and provides a method for synthesizing 2-methyl-3, 4, 5-trifluorophenol, which comprises the following steps: S1, carrying out chloromethylation reaction on 3, 4, 5-trifluorobromobenzene serving as a raw material under the action of paraformaldehyde and chlorosulfonic acid to obtain 2-chloromethyl-3, 4, 5-trifluorobromobenzene; s2, the 2-chloromethyl-3, 4, 5-trifluorobromobenzene is subjected to a reduction reaction, and 2-methyl-3, 4, 5-trifluorobromobenzene is obtained; s3, 2-methyl-3, 4, 5-trifluorobromobenzene is subjected to a substitution reaction, hydrolysis, crystallization and filtration, and 2-methyl-3, 4, 5-trifluorophenylboronic acid is obtained; s4, 2-methyl-3, 4, 5-trifluorophenylboronic acid is subjected to an oxidation reaction, and 2-methyl-3, 4, 5-trifluorophenol is obtained; the crystallization solvent is composed of an ether solvent and water. According to the technical scheme, the problems of high cost and low yield in synthesis of 2-methyl-3, 4, 5-trifluorophenol in related technologies are solved.

A synthesis method of 2-chloro-4-bromobenzonitrile comprises the following steps: S1, adding methylchloroaniline and hydrobromic acid into a solvent a, dropwise adding a sodium nitrite solution, rapidly cooling to room temperature after the reaction is completed, and filtering to obtain a compound I; s2, adding the compound I, bromine and a solvent b into a reaction kettle, stopping heating after the reaction is completed, naturally cooling to room temperature, and filtering to obtain a compound II; s3, adding the compound II, hydroxylamine hydrochloride and sodium hydroxide into the reaction kettle, stopping heating after the reaction is completed, naturally cooling to room temperature, and filtering to obtain a compound III; s4, adding the compound III into thionyl chloride and a solvent c, stopping heating after the reaction is completed, naturally cooling to room temperature, and filtering to obtain 2-chloro-4-bromophenoxybenzene; and (S5) carrying out cyclohexane refining on the 2-chloro-4-bromobenzonitrile. According to the synthetic method of the 2-chloro-4-bromobenzonitrile, the 2-chloro-4-bromobenzonitrile is synthesized through four-step reaction of diazotization, hydroformylation, oximation and nitrilation, and the method is simple in process, stable in quality, low in energy consumption and easy to produce.

The present invention relates to a method for synthesizing the fluxapyroxad intermediate trifluoronitro - biphenyl, belonging to the technical field of organic synthesis. The method process includes the following: Step1: Under nitrogen protection, add 3,4,5 - trifluorobromobenzene, o - nitrophenylboronic acid, a catalyst, a cocatalyst, a base and a solvent into a reaction flask. After addition, carry out a heat - preservation reaction; Step2: After the reaction is completed, through phase separation, the organic phase is concentrated to obtain 3’,4’,5’ - trifluoro - 2 - nitrobiphenyl. In the present invention, compared with the traditional method for synthesizing trifluoronitro - biphenyl, the method for synthesizing trifluoronitro - biphenyl directly uses 3,4,5 - trifluorobromobenzene and o - nitrophenylboronic acid as raw materials, avoiding the production steps of preparing 3,4,5 - trifluorobenzeneboronic acid from 3,4,5 - trifluorobromobenzene through multiple steps. Moreover, it can effectively improve the yield, has a high raw material utilization rate, and the preparation method of o - nitrophenylboronic acid is simple, which can effectively reduce the reaction cost. The reaction route is shorter, simpler and more efficient, the reaction conditions are mild, and it has high industrial application value.

The invention belongs to the technical field of fine chemical engineering, and particularly relates to a method for preparing deuterated 1, 3-dibromobenzene by adopting a hydrogen-deuterium exchange method, which comprises the following steps of: in the presence of a catalyst and alkali, carrying out hydrogen-deuterium exchange reaction on 1, 3-dibromobenzene and heavy water in an organic solvent, and further purifying to obtain the deuterated 1, 3-dibromobenzene. The preparation method utilizes a hydrogen-deuterium exchange process to synthesize deuterated 1, 3-dibromobenzene in one step, and has the advantages of simplicity and convenience in operation, high safety, high yield, good economic applicability, easiness in purification and the like.

The invention belongs to the technical field of medicine preparation, and particularly relates to a fenoprofen calcium preparation method which comprises the following steps: 1) m-hydroxyacetophenone and bromobenzene generate an intermediate 1, namely m-phenoxyacetophenone under the action of alkali and cuprous iodide; 2) reacting the intermediate 1 with ethyl chloroacetate under the action of strong base, and then performing hydrolysis and decarboxylation reaction to generate an intermediate 2, namely 2-(3-phenoxy phenyl) propionaldehyde; the invention discloses a preparation method of fenoprofen calcium, which comprises the following steps: (1) preparing fenoprofen, (2) preparing fenoprofen, (3) carrying out oxidation reaction on an intermediate 2 to obtain fenoprofen, (4) reacting fenoprofen with a sodium hydroxide solution to obtain fenoprofen sodium, and (5) salifying fenoprofen sodium with a calcium chloride solution to obtain fenoprofen calcium.

The application discloses a synthesis method of aromatic aldehyde, comprising the following steps: under inert atmosphere, a compound shown in formula I and a compound shown in formula II are reacted in an organic solvent containing a photocatalyst, a nickel catalyst, a ligand, a base and water under blue light irradiation to obtain aromatic aldehyde shown in formula III; formula I, formula II and formula III are structures as follows, ring A is selected from benzene, pyridine, thiophene, furan, pyridazine, indazole, indole, isoquinoline, quinoline, naphthalene, benzothiophene, dibenzofuran or dibenzothiophene; the application generates formyl radicals under the nickel synergistic photo-oxidation and reduction catalytic condition, and the formylation of bromobenzene and its derivatives is realized in a simple and efficient one-pot way, aromatic aldehyde is constructed, and the reaction has the characteristics of cheap and easily available raw materials, mild reaction conditions, controllable synthesis process, high separation yield / yield, green environmental protection, wide substrate applicability and the like.

The invention belongs to the technical field of pesticides, and particularly relates to a synthesis method of 2, 6-difluorostyrene. According to the method, 2, 6-difluorobromobenzene is adopted as a Grignard reagent, so that the reaction is mild; the raw materials are easy to obtain, the production cost is low, the conversion rate is high, the two-step total yield can reach 85% or above, and the raw materials are completely converted; the product is easy to separate, water washing, liquid separation and distillation are performed after the reaction is completed, excessive acetaldehyde directly enters a water phase, and the product is left in an organic phase.

The present invention relates to a one-pot synthesis method of the fluxapyroxad intermediate 3',4',5'-trifluoro-2-nitrobiphenyl, belonging to the technical field of organic synthesis. The method process includes the following steps: Step 1: Under nitrogen protection, add magnesium chips, a catalyst and a solvent to a reaction flask, and then dropwise add a mixed solution of 3,4,5-trifluorobromobenzene, o-chloronitrobenzene and borate ester. After the dropping is completed, keep the reaction under heat preservation; Step 2: After the reaction is completed, acidify and wash with 10% dilute hydrochloric acid, and after phase separation, the obtained organic phase is concentrated under reduced pressure to obtain 3',4',5'-trifluoro-2-nitrobiphenyl. In the present invention, compared with the traditional synthesis method of the fluxapyroxad intermediate, the synthesis method of the present fluxapyroxad intermediate does not need to prepare 3,4,5-trifluorophenylboronic acid first, but directly uses 3,4,5-trifluorobromobenzene and o-chloronitrobenzene as raw materials. The "one-pot" synthesis method has a short reaction route, high raw material utilization rate, and can greatly reduce the raw material cost.

The invention relates to a preparation method of a high-performance imidazolyl polyionic liquid membrane, and belongs to the technical field of ionic membranes. The method comprises the following steps: by taking N-methyl pyrrolidone as a solvent, reacting 2-phenylbenzimidazole or 2, 4, 5-triphenylimidazole with 4, 4-difluorodiphenyl sulfone, 1, 4-dibromobenzene, 4, 4-dibromodiphenyl or 4, 4-dibromodiphenyl terphenyl in a hydrothermal reaction kettle, washing and drying to obtain a product I; under the catalysis of super organic acid, reacting the product I with biphenyl or p-terphenyl and N-methyl-4-piperidone, washing and drying; adding methyl iodide in an alkaline environment for reaction, and washing and drying to obtain polyion liquid; and dissolving in dimethyl sulfoxide, coating on a glass plate, and drying to prepare the film. The polyionic liquid membrane prepared by the method has more ionic sites, and the ionic conductivity is remarkably improved. Tests show that the stability of the membrane is almost unchanged after 1500 hours under the conditions of 80 DEG C and 1M KOH, the wet mechanical property reaches 60 MPa or above, and the membrane has high chemical and mechanical stability and wide application prospects.

The invention discloses a preparation method of pinoxaden, and belongs to the field of organic synthesis. The synthesis method comprises the following synthesis steps: (1) reacting dimethyl malonate with hydrazine hydrate under the action of alkali to generate pyrazolidine-3, 5-diketone; (2) carrying out cyclization on the pyrazolidine-3, 5-diketone and diethylene glycol dimethanesulfonate to generate dihydro-1H-pyrazolo [1, 2-d] [1, 4, 5] oxadiaze-7, 9 (2H, 8H)-diketone; (3) carrying out a coupling reaction on the dihydro-1H-pyrazolo [1, 2-d] [1, 4, 5] oxadiaze-7, 9 (2H, 8H)-diketone and 2, 6-diethyl-4-methyl bromobenzene, so as to obtain 8-(2, 6-diethyl-4-methyl phenyl)-tetrahydropyrazolo [1, 2-d] [1, 4, 5] oxadiaze-7, 9-diketone; and (4) carrying out a reaction on the 8-(2, 6-diethyl-4-methylphenyl)-tetrahydropyrazolo [1, 2-d] [1, 4, 5] oxadiaza-7, 9-diketone and pivaloyl chloride to generate the pinoxaden. The method disclosed by the invention is simple to operate, mild in reaction condition and suitable for industrial mass production.

The invention discloses a preparation method of a key intermediate epoxide of rubaburon, and belongs to the technical field of organic synthesis. The method comprises the following steps: (1) adding a solvent, 2-(2-bromophenyl) thiophene and a basic catalyst into a reaction container, dropwise adding glycidol while stirring, and continuously reacting after dropwise adding until the 2-(2-bromophenyl) thiophene is completely reacted; and (2) cooling and filtering to remove salt, concentrating filtrate to be dry, adding methanol, heating and dissolving, cooling and crystallizing, filtering and drying to obtain the 2-((2-thiophene-2-yl) phenoxy) methyl) ethylene oxide. According to the invention, new raw materials and a new synthetic route are selected to prepare the key intermediate epoxide of the rubaburon, the production process is simple, and the key intermediate epoxide of the rubaburon, which is higher in yield, less in side reaction and lower in cost, is obtained.