21 results about "Butyl lithium" patented technology

The invention provides a kilogram-level preparation method of an organic photoelectric conjugated tin reagent, and belongs to the field of organic synthesis and organic photoelectric materials. The method comprises the following steps: in a dry 20L reaction device, dissolving a conjugated thiophene compound in tetrahydrofuran, keeping nitrogen positive pressure protection, dropwise adding a tetrahydrofuran solution of n-butyllithium and a tetrahydrofuran solution of trimethyltin chloride in a low-temperature reaction system, stirring for reaction, after the reaction is completed, standing for phase splitting, collecting an organic phase, drying, and concentrating filtrate to obtain the conjugated thiophene compound. And recrystallizing to obtain the organic photoelectric conjugated tin reagent. According to the method, efficient macro preparation of various conjugated tin reagents can be achieved, 1-1.2 kg of target products can be prepared through single-batch reaction, and the method has the advantages of being high in yield, easy and convenient to operate, low in cost, good in environmental friendliness and the like.

The invention discloses a kilogram-level preparation method of an organic photoelectric conjugated boron reagent, and belongs to the technical field of organic synthesis and organic photoelectric materials. A kilogram-level preparation method of an organic photoelectric conjugated boron reagent comprises the following steps: uniformly mixing aryl halide and tetrahydrofuran in an inert gas atmosphere to obtain a mixed system 1; placing the mixed system 1 in a liquid nitrogen environment, then dropwise adding a THF solution of n-butyllithium, and stirring to obtain a mixed system 2; and adding a boric acid ester compound into the mixed system 2 for reaction, and finally performing purification treatment to obtain a target product, namely the organic photoelectric conjugated boron reagent. The preparation method of the conjugated boron reagent is efficient, safe and capable of achieving large-scale production, has the advantages of being easy and convenient to operate, low in cost, high in yield, good in purity and the like, is suitable for various benzene series, thiophene, fluorene and other substrates, achieves kilogram-level stable preparation, solves the amplification problem, improves supply chain autonomy, and is suitable for industrial production. The application requirements in the fields of high-end medicines and materials are met.

The invention provides a phenyl phosphonic acid bis (o-isocyano-phenol) ester ligand which is prepared by the following steps: in an inert gas atmosphere, mixing a compound benzoxazole with anhydrous tetrahydrofuran, cooling to-95 to-65 DEG C, adding an n-butyllithium solution dissolved in an organic solvent, stirring at-95 to-65 DEG C for 0.5-4 hours, adding diphenylphosphoryl chloride, stirring at room temperature for 8-10 hours, filtering, washing, and drying to obtain the phenyl phosphonic acid bis (o-isocyano-phenol) ester ligand. Carrying out post-treatment on the obtained reaction liquid to obtain a phenyl phosphonic acid bis (o-isocyano phenol) ester ligand; compared with the most common organic dye photosensitizer, the copper-based photosensitizer prepared from the phenyl phosphonic acid bis (o-isocyano-phenol) ester ligand overcomes the defect that the catalytic activity of the organic dye photosensitizer is rapidly reduced under long-term illumination, and in addition, the organic dye photosensitizer is easy to generate an aggregation-induced quenching effect; the photosensitizer disclosed by the invention does not generate an aggregation-induced quenching effect; compared with an iridium complex photosensitizer which is commonly used at present, the cuprous photosensitizer provided by the invention is more environment-friendly.

The application belongs to the technical field of organic synthesis, and particularly relates to a kind of bromine-containing isoindoline-1-ketone compound and preparation method thereof.The preparation method of the bromine-containing isoindoline-1-ketone compound uses commercially available aldehyde-derived imine as raw material, is reacted with aryl bromide oxazoline compound under butyl lithium condition, and then is subjected to acid-mediated cascade cyclization process, to efficiently construct isoindoline-1-ketone skeleton.The isoindoline-1-ketone compound can be directly used as an organic catalyst, the N-H functional group remaining in the structure of the isoindoline-1-ketone compound has reactivity, can be coupled with other bioactive molecules as a key connection site, to construct functional derivatives, the amide carbonyl group thereof can be further reduced, to be converted into pyrrolidine structural unit, and the structure itself can be used as a catalytically active center, to expand its application in the field of catalysis.

The invention discloses a lithium ion conductor type lithium supplement agent, a composite positive electrode material, a positive electrode plate and a battery, and belongs to the technical field of batteries. The lithium ion conductor type lithium supplement agent comprises the following raw materials: a strong reduction organic lithium reagent and an inorganic solid electrolyte, the strong reduction organic lithium reagent comprises at least one of n-butyl lithium, tert-butyl lithium and naphthalene lithium; and the inorganic solid electrolyte is Li < 1.3 > Al < 0.3 > Ti < 1.7 > (PO4) 3. The lithium ion conductor type lithium supplement agent is an over-lithiated inorganic solid electrolyte, and no extra gas is generated when the lithium ion conductor type lithium supplement agent is used as the lithium supplement agent; after the lithium supplement function of the lithium supplement agent is exerted, residues still have good ion conduction capability, the cycle performance of the material can be improved, the capacity of the whole battery is effectively improved, the cycle life of the whole battery is effectively prolonged, and the lithium supplement method for the lithium ion battery is simple, convenient and efficient.

The invention provides an organic dilithium compound, a preparation method thereof and hydroxyl-terminated liquid polybutadiene rubber. The preparation method comprises the following steps: in a protective atmosphere, mixing a solvent, a bromine-containing vinyl benzene compound A, a catalyst and piperazine, and carrying out reaction and post-treatment to obtain a product S1; under a protective atmosphere, mixing the product S1, cyclohexane and alkyl lithium, and reacting to obtain an organic dilithium compound; the molar ratio of the bromine-containing vinyl benzene compound A to the piperazine is (2-3): 1; the molar ratio of the product S1 to lithium alkyl is 1: (2.5-3.5); the lithium alkyl comprises one of n-butyl lithium, sec-butyl lithium and tert-butyl lithium; by mass, the use amount of the catalyst is 1%-5% of that of the bromine-containing vinyl benzene compound A. The organic dilithium compound has good solubility and activity in a non-polar solvent, and when the organic dilithium compound is applied to preparation of hydroxyl-terminated liquid polybutadiene rubber through anionic polymerization, butadiene monomer polymerization can be initiated at two ends, and the phenomenon of false gel is overcome.

The application discloses a method for synthesizing a carbazole derivative, which does not need transition metal catalysis, directly realizes intramolecular C-C bond coupling reaction by reaction of a photoinduced diarylamine with a Grignard reagent or n-butyl lithium, and obtains the carbazole derivative. The reaction system is simple, the operation is simple, the reaction condition is mild, and the yield is good; the traditional noble metal catalyst is avoided; and the method provides a new method for green and efficient synthesis of the carbazole derivative without transition metal catalysis for medicines, pesticides and organic materials.

The invention discloses a synthesis method of 2, 2 '-bis (trifluoromethyl)-4, 4', 5, 5 '-biphenyl dianhydride, which comprises the following steps: by taking 3-nitro-4-methylbenzotrifluoride as an initial raw material, firstly carrying out hydrogenation coupling to obtain a first intermediate 2, 2'-dimethyl-5, 5 '-bis (trifluoromethyl) hydrogenated azobenzene, then carrying out transposition rearrangement to obtain a second intermediate 2, 2'-bis (trifluoromethyl)-5, 5 '-dimethyl benzidine, and then carrying out condensation reaction to obtain 2, 2'-bis (trifluoromethyl)-4, 4 ', 5, 5'-biphenyl dianhydride, thereby obtaining the 2, 2 '-bis (trifluoromethyl)-4, 4', 5, 5 '-biphenyl dianhydride. The preparation method comprises the following steps: reacting 2, 2 '-bis (trifluoromethyl)-4, 4', 5, 5 '-dimethyl biphenyl dinitrile to obtain a third intermediate 2, 2'-bis (trifluoromethyl)-5, 5 '-dimethyl biphenyl dinitrile, and carrying out hydrolysis, oxidation and anhydride formation to obtain 2, 2'-bis (trifluoromethyl)-4, 4 ', 5, 5'-biphenyl dianhydride. The synthesis method provided by the invention has the advantages of cheap and easily available initial raw materials, no need of using expensive iodine reagent and butyl lithium, low production cost, mild reaction conditions, low energy consumption, environmental friendliness and high total yield, and is suitable for large-scale industrial production.

This invention discloses a method for preparing a supercapacitor based on a molybdenum disulfide thin film electrode, comprising the following steps: (1) immersing molybdenum disulfide powder in a butyllithium solution to complete a chemical lithiation reaction; after the reaction, washing the resulting lithiation product and then adding it to deionized water for ultrasonic exfoliation; centrifuging after ultrasonic exfoliation to obtain a molybdenum disulfide nanosheet suspension; the suspension is vacuum filtered to form a film to obtain a re-stacked molybdenum disulfide thin film electrode; (2) adding cesium salt to deionized water and stirring at room temperature until completely dissolved to obtain a cesium salt aqueous solution, which serves as the aqueous electrolyte for the supercapacitor; (3) assembling the re-stacked molybdenum disulfide thin film electrode from step (1) and the cesium salt aqueous solution from step (2) into a supercapacitor under normal atmospheric conditions. The supercapacitor of this invention possesses excellent high-rate charge-discharge performance and maintains good capacitance retention even under high-current charge-discharge conditions.

The invention discloses a preparation method of a di (ketene glycol) monomer (DETOSU), which adopts a DETOSU precursor as a raw material, selects LiHMDS and other specific alkali reagents, adopts a charging sequence of firstly adding the DETOSU precursor and then adding the alkali reagents, reduces the content of unilateral heterogeneous byproducts to a controllable range on the basis of ensuring medium and above reaction yield, and has the advantages of mild reaction conditions, high yield, low cost and high yield. The adoption of an n-butyllithium flammable and explosive reagent or a pentacarbonyl iron highly toxic product is avoided, and the method is more suitable for industrial large-scale production.

This invention discloses a novel bisphosphine ligand, its preparation method, and its applications, belonging to the field of organometallic catalysis technology. The invention utilizes a chemical synthesis method, starting with ferrocene or 1,1'-dimethylferrocene, followed by butyl lithiation (or bromination), introduction of an aldehyde group (or palladium-catalyzed hydromethyl esterification), aldehyde reduction (or ester reduction), halogenation of the hydroxyl group (or bis-OTf oxidation), and condensation with a lithium phosphine reagent (or direct Herrman-Beller catalytic coupling), to obtain the novel bisphosphine ligand based on the ferrocene framework. The catalytic complex of this bisphosphine ligand and palladium exhibits excellent catalytic activity and selectivity in the alkoxycarbonylation reactions of terminal alkenes, internal alkenes, and polysubstituted alkenes.

The utility model provides a microchannel continuous flow device for preparing deuterated phenylboronic acid, which relates to the technical field of microchannel reactors, and comprises a material storage system, a feeding system, a series microchannel reaction module and a continuous extraction system, the material storage system comprises a bromobenzene-tetrahydrofuran solution storage device, an n-butyllithium-n-hexane solution storage device, a triisopropyl borate-tetrahydrofuran solution storage device, a hydrochloric acid aqueous solution storage device, an ethyl acetate storage device and a saturated sodium chloride aqueous solution storage device; the series micro-channel reaction module comprises a first plate type micro-channel reactor, a second plate type micro-channel reactor and a third plate type micro-channel reactor which are sequentially communicated in series. The method has the advantages that multi-step continuous reaction can be completed, the reaction is fast, reaction process control points are controlled in a targeted manner, and side reaction can be well inhibited, so that the yield of the deuterated phenylboronic acid is increased, and continuous and efficient synthesis of the target product deuterated phenylboronic acid is realized.

The application provides a preparation method and device system of dialkylamino metal halide and diimino bis(dialkylamino) metal complex, and the device system corresponds to the preparation method. The preparation method promotes the reaction of the formation of the favorable product, reduces the occurrence of the side reaction, avoids the defects of the introduction of metal impurities by using n-butyl lithium, avoids the generation of lithium salt and other components which are inconvenient for subsequent separation, and facilitates the purification of the product. Moreover, the dialkylamino metal halide and diimino bis(dialkylamino) metal complex prepared by the application meet the purity requirements of the precursor material in integrated circuit manufacturing.

The application belongs to the technical field of photocatalysis, and particularly relates to a benzylamine lead iodine / molybdenum disulfide photocatalyst, a preparation method and application thereof, and a photocatalytic overall water splitting method. The preparation method comprises the following steps: mixing benzylamine and hydroiodic acid, and evaporating a solvent to obtain PMAI; dissolving lead iodide in hydroiodic acid, adding PMAI, crystallizing after heating and keeping warm, cooling, and separating to obtain PMA2PbI4 and a PMA2PbI4 saturated solution; soaking MoS2 powder in a n-butyl lithium solution, separating and washing a precipitate, and ultrasonically peeling to obtain MoS2 nanosheets; adding PMA2PbI4 and the MoS2 nanosheets to the PMA2PbI4 saturated solution, reacting after heating, cooling, and collecting a precipitate to obtain the benzylamine lead iodine / molybdenum disulfide photocatalyst. The benzylamine lead iodine / molybdenum disulfide photocatalyst can stably produce hydrogen in a dilute HI solution and has excellent activity, and can be placed in the same reaction system with an oxygen production catalyst to realize photocatalytic overall water splitting.

The invention relates to the technical field of polymer functional materials, and discloses a preparation method and system of bifunctional ion exchange resin for petrochemical wastewater treatment.The method comprises the steps that N, N-diethylbenzamide functionalized polystyrene divinylbenzene resin is used as guiding resin; carrying out ortho-position metallization on the guide resin through sec-butyllithium by adopting a swelling metallization coupling sequential control process; then introducing sulfur dioxide and introducing a sulfinate precursor; and finally, carrying out one-step series conversion in an acidic hydrogen peroxide solution, oxidizing the sulfinate precursor into a sulfonic acid group, and hydrolyzing the N, N-diethylbenzamido into a carboxylic acid group. According to the invention, through ortho-orientation and tandem conversion, ortho-introduction of a sulfonic acid group and a carboxylic acid group on the same benzene ring according to a stoichiometric ratio of 1: 1 is realized. And the homogeneity and efficiency of the functionalization reaction are improved by adopting a swelling metallization coupling time sequence control process. The overall reaction conditions are mild, and the mechanical and thermal stability of a resin skeleton is effectively maintained.

The invention relates to a method for preparing (cyclopentadienyl) tris (dimethylamino) zirconium by using nuclear magnetic control, which comprises the following steps: S1, carrying out heating reflux reaction on zirconium tetrachloride, cyclopentadiene and dimethylamine in the presence of n-butyllithium and n-hexane, and after reacting for a certain time, taking supernate to detect a nuclear magnetic hydrogen spectrum; s2, calculating the ratio a of the integral area of the characteristic peak A to the integral area of the characteristic peak B according to the nuclear magnetic hydrogen spectrum, judging whether a is in a target range or not, if a is in the target range, terminating the reaction, separating a liquid phase, distilling and collecting a crude product; and if a value is greater than the maximum value of the target range, adding cyclopentadiene into the reaction system to continue the reaction, and if a value is less than the minimum value of the target range, continuing the reaction until the ratio of the integral area of the characteristic peak A to the integral area of the characteristic peak B in the nuclear magnetic hydrogen spectrum of the reaction supernatant is within the target range, terminating the reaction, separating the liquid phase, distilling and collecting a crude product. The method can effectively improve the safety of the production process, the raw material conversion rate and the product purity.

The invention provides a novel method for synthesizing an ipidakrin intermediate, and belongs to the technical field of medical intermediates. According to the method, adiponitrile is used as a raw material, a KF-Al2O3 / DMF system is adopted, the target product 1-amino-2-cyano-1-cyclopentene is directly obtained through a microfluid technology and a one-step reaction, the production process is greatly simplified, the yield of 1-amino-2-cyano-1-cyclopentene is much higher than that of 1-amino-2-cyano-1-cyclopentene obtained through a traditional synthesis route, potassium tert-butoxide does not need to be used in the whole reaction process, and the method is suitable for industrial production. And high-activity substances such as butyl lithium and the like are simple and convenient in post-treatment. The final product is white crystalline powder; and the product is odorless and tasteless and has very high purity. By adopting the improved synthesis route, the method has the advantages of greatly improving the yield, reducing the cost, improving the safety, saving energy and the like, meets the modern chemical production requirements of green reaction, and also meets the dual-carbon target proposed by the country.

The invention provides an aza-adamantane quaternary ammonium salt phosphine ligand as well as a preparation method and application thereof, and belongs to the technical field of organic synthesis. The preparation method comprises the following steps: under the protection of inert atmosphere, mixing a phosphine-containing compound with a first organic solvent, adding an n-butyllithium solution into the obtained phosphine-containing compound solution, carrying out deprotonation reaction at low temperature, mixing the obtained phosphine-lithium intermediate with dichloromethane, and carrying out chloromethylation reaction to obtain a chloromethyl phosphine compound; mixing the chloromethyl phosphine compound, aza-adamantane and a second organic solvent, and carrying out quaternization reaction to obtain various substituted aza-adamantane quaternary ammonium salt phosphine ligands; the azaadamantane quaternary ammonium salt phosphine ligand can simultaneously exert the space and charge advantages of azaadamantane and the electron adjustability of phosphine, shows better thermal stability and solvent compatibility in a catalytic system, and can be used for constructing a novel bifunctional phase transfer catalyst or a phosphine ligand precursor.

The present application relates to a kind of preparation method of tetra (dimethylamino) tin, belong to the technical field of organic synthesis.The preparation method of the present application includes the following steps: S1: adding solvent to metal hydride, to obtain suspension liquid;S2: drop anhydrous tin tetrachloride to suspension liquid, reaction obtains reaction liquid;S3: dimethylamine is introduced into reaction liquid, stirring reaction, to obtain mixture;S4: mixture is subjected to low boiling under reduced pressure, reduced pressure distillation, rectification obtains the tetra (dimethylamino) tin of the present application.The preparation method of the present application replaces active high and difficult to control n-butyl lithium with metal hydride, and the activity of metal hydride is greatly reduced, and violent reaction does not occur, so the safety is greatly improved, and metal hydride can replace n-butyl lithium as acid binding agent and participate in reaction, promote reaction, to obtain target product, and metal hydride does not react with product, so that cost is greatly reduced, greatly improve the safety, be conducive to large-scale preparation.

The application discloses a preparation method of lifitegrast intermediate benzofuran-6-carboxylic acid, and relates to the technical field of medicines, and comprises the following steps: S1, ring-closing reaction of a compound of formula (I) with acetic anhydride under heating to obtain a compound of formula (II); S2, catalytic reaction of the compound of formula (II) with a compound of formula (III) under catalysis of n-butyl lithium to obtain a compound of formula (IV), and then first hydrolysis reaction under alkaline conditions to obtain benzofuran-6-carboxylic acid. The preparation method of the lifitegrast intermediate benzofuran-6-carboxylic acid is low in cost, high in yield and mild in reaction conditions.

The invention discloses a method for preparing transition metal chalcogenide crystals or nanosheets. The method for preparing the nanosheet comprises the following steps: removing intercalated metal from a metal intercalated transition metal chalcogenide crystal or removing residual metal after soaking the metal intercalated transition metal chalcogenide crystal in a lithium ion solution; and then ultrasonically dispersing in water to obtain an MX2 nanosheet dispersion liquid. The preparation method of the metal-intercalated transition metal chalcogenide crystal comprises the following steps: mixing a transition metal source precursor and A (HX) n, carrying out high-temperature reaction, and rapidly cooling; in A (HX) n, A is metal and is selected from at least one of alkali metal and alkaline earth metal; x is a chalcogenide element; the temperature of the high-temperature reaction is not less than 400 DEG C. According to the method provided by the invention, butyl lithium and other high-risk organic lithium reagents are not needed, the reaction time is short, the yield is high, and gram-level to kilogram-level amplified preparation can be realized.