59 results about "N-Butyllithium" patented technology

The invention discloses chain end modified liquid rubber, mixed rubber, a preparation process, a tire and a vehicle, and belongs to the technical field of liquid rubber and manufacturing thereof. According to the liquid rubber, butadiene monomers and a chain transfer agent are added in batches in the preparation process, negative ion active centers are frequently transferred to the chain transfer agent from the tail end of a polybutadiene-based lithium active chain to form new initiation growth centers, then newly introduced butadiene monomers are initiated to grow, the dosage of an n-butyllithium initiator is remarkably reduced, and the stability of the liquid rubber is improved. The production cost is greatly reduced, the generation of sewage is greatly avoided, the monomer concentration of the final rubber product can reach about 80 percent by weight, the productivity is improved, and large-scale production is facilitated; the rubber also enables the filler to have good dispersibility, and has good compatibility with base rubber such as styrene butadiene rubber, natural rubber and the like.

The utility model provides an n-butyllithium taking bottle which comprises a bottle body and a bottle cap and is characterized in that the bottle body is composed of an inner layer structure and an outer layer structure, an air inlet pipe and a liquid outlet pipe are arranged on the bottle cap, an air inlet valve is arranged on the air inlet pipe, a liquid outlet valve and a buckle are arranged on the liquid outlet pipe, and the liquid outlet pipe and a feeding pipe are connected through the buckle. And an air bag and a feeding needle are arranged on the feeding pipe. The n-butyllithium taking device is connected with an air inlet and liquid outlet device, so that the n-butyllithium taking device is safer when n-butyllithium is taken. When the n-butyllithium bottle topples over or falls off accidentally, the two-layer structure can protect the bottle body from being broken, reagents in the bottle are not prone to being leaked, and accidents are reduced.

The invention relates to a method for preparing (cyclopentadienyl) tris (dimethylamino) hafnium by using nuclear magnetic control, which comprises the following steps: S1, carrying out heating reflux reaction on hafnium 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 belongs to the technical field of chemical synthesis of semiconductor materials, and particularly relates to a synthesis method of tetra (dimethylamino) titanium, which comprises the following steps: (1) reacting titanium tetrachloride with dimethylamine to generate an intermediate TiClx [N (CH3) 2] 4-x, where x is an integer from 0 to 4; (2) reacting dimethylamine with an organic metal lithium reagent to synthesize lithium dimethylamino (LiN (CH3) 2); and (3) reacting the intermediate obtained in the step (1) with lithium dimethylamino obtained in the step (2) to obtain tetra (dimethylamino) titanium. By adopting a step-by-step reaction strategy, the dependence on expensive n-butyllithium is fundamentally reduced, the raw material cost is remarkably reduced, meanwhile, the reaction process is optimized by generating an intermediate, the product yield is greatly improved, the generation of byproducts is effectively reduced, and the product purity is improved.

This invention relates to a simple method for modifying β-ketoimine ligand precursors, wherein L... Ph The reaction involves a lithium compound with H2 solution; then a haloalkane is added for C-C coupling; followed by the addition of an acid solution to complete the modification of the β-ketoimine ligand precursor, yielding a terminally alkylated ketoimine. This invention relates to a simple method for modifying β-ketoimine ligand precursors, specifically involving the removal of the proton at the α-position of the β-ketoimine ligand precursor from commercially available n-butyllithium to form a deprotonated β-ketoimine lithium compound, followed by C-C coupling to achieve alkylation at the α-position of the ketocarbonyl group, thus providing a convenient modification of the β-ketoimine ligand precursor.

The application discloses a preparation method of triethyl indium, and relates to the technical field of metal organic source synthesis, wherein a commonly used indium source is mainly trimethyl indium; the trimethyl indium is in a solid state at normal temperature, and is easy to cause the solid indium source to be easy to be hardened and to have excessive residues; when the solid indium source is used in a machine, the concentration output stability is worse than that of a liquid source; the liquid indium source will become an important indium source in the future; the operation method of the triethyl indium in preparation is more complicated; and the purity of the triethyl indium prepared by purification cannot reach a better ideal state. In the application, n-butyllithium and ethyl iodide are reacted under the protection of inert gas, then the reaction product is reacted with indium chloride to generate triethyl indium; the whole operation is simple, raw materials are easy to obtain, and the product has high purity; under the protection of inert gas, the interference of other solution reagents in the preparation process is reduced; therefore, high-quality triethyl indium raw materials can be purified and processed.

A method for preparing high-purity lithium sulfide by using industrial-grade butyllithium includes the following steps: step A: under an inert gas condition, thoroughly mixing 1.5-2.5 g of lithium chloride, 0.5 L of an industrial-grade n-butyllithium solution (2.5 mol / L) and 1.5-2.5 L of n-hexane to obtain a mixed solution, and charging the mixed solution into a sealed container; step B: under the sealed condition, firstly introducing H2S gas into a gas-washing bottle through a submerged pipe at a rate of 10.5 L / h, then introducing into the mixed solution through the submerged pipe, controlling the reaction temperature at 25-40° C., and continuously stirring for reaction for 4-6 h to obtain a reaction slurry; and step C: under an inert gas condition, filtering the reaction slurry with a G3 sand core funnel to obtain a crude lithium sulfide solid wet material.

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 synthesis method of a high-purity hafnium-zirconium metal complex precursor, and belongs to the technical field of high-dielectric-constant materials for super-large-scale integrated circuits. According to the method, hafnium tetrachloride or zirconium tetrachloride is used as a metal source and sequentially reacts with dialkylamine, n-butyllithium and an alkyl magnesium halide Grignard reagent through a one-pot method in a high-purity inert atmosphere, an intermediate does not need to be separated, and a target precursor is obtained after filtration, washing and rectification. The method is simple and convenient in process operation, mild in reaction condition and low in energy consumption; the raw materials are wide in source and low in price, the product yield reaches 82%-88%, and the metal purity is stabilized to be 6N; when the precursor is used for preparing a hafnium oxide / zirconium thin film through atomic layer deposition (ALD), the thickness of the thin film reaches 14.3 nm under 100 cycles, the non-uniformity is smaller than or equal to 0.90%, the requirement of a gate dielectric layer of a super-large-scale integrated circuit for a high-purity and high-efficiency precursor can be met, and the precursor is suitable for industrial amplification production.

The invention belongs to the technical field of deuterated organic chemical synthesis, and particularly relates to a synthesis method of deuterated 9-phenyl anthraceneboronic acid-D8, which comprises the following steps of: 1, halogenation reaction: reacting 9-phenyl anthracene-D9, bromo-succinimide (NBS) and triethylamine (TEA) in dichloromethane at low temperature to generate an intermediate 9-phenyl-10-bromoanthracene-D8; step 2, carrying out nucleophilic reaction of forming carbon negative by pulling out bromine with strong in a low-temperature environment of-65 DEG C to-70 DEG C, reacting n-butyllithium with the intermediate 9-phenyl-10-bromoanthracene-D8 in 2-methyltetrahydrofuran to generate 9-phenyl anthracene lithium; then triisopropyl borate is added for a boronation reaction, and the 9-phenyl anthracene boric acid-D8 is obtained after hydrochloric acid hydrolysis and purification. The purity of the deuterated 9-phenyl anthracene boric acid-D8 is greater than or equal to 99.8%, the deuteration rate is greater than or equal to 98%, and the deuterated 9-phenyl anthracene boric acid-D8 is suitable for being used as

The invention belongs to the technical field of ceramic precursors, and particularly relates to a silicon-boron-carbon-nitrogen ceramic precursor with a main chain containing alkynyl and a preparation method of the silicon-boron-carbon-nitrogen ceramic precursor. Comprising the following steps: (1) dropwise adding an n-butyllithium solution into an ether solvent, stirring, continuously dropwise adding trichloroethylene, and reacting to obtain an alkynyl dilithium salt turbid solution; (2) adding boron trichloride into the alkynyl dilithium salt turbid solution to carry out primary dechlorination polycondensation reaction, and dropwise adding dichlorosilane to carry out secondary dechlorination polycondensation reaction after the reaction is completed; (3) adding hexamethyldisilazane into the system in the step (2) to carry out an end-capping reaction, collecting supernate after the reaction is finished, and distilling at normal pressure to remove the solvent, so as to obtain a silicon-boron-carbon-nitrogen ceramic precursor crude product; and (4) dissolving the silicon-boron-carbon-nitrogen ceramic precursor crude product in an organic solvent, carrying out dialysis treatment, and carrying out atmospheric distillation on the solution in a dialysis membrane to remove the solvent so as to obtain the silicon-boron-carbon-nitrogen ceramic precursor with the main chain containing alkynyl, and the ceramic yield of the silicon-boron-carbon-nitrogen ceramic precursor in the high-temperature ceramization process can reach more than 70%.

The application relates to a solution polymerization styrene-butadiene SSBR rubber and a preparation method thereof, and belongs to the technical field of solution polymerization styrene-butadiene rubber. The preparation raw materials of the solution polymerization styrene-butadiene SSBR rubber include 25-35 parts of styrene, 30-40 parts of butadiene, 75-85 parts of a cyclohexane solution, 0.5-1.5 parts of a polarity regulator, 2-5 parts of an atomization terminator and 0.5-2.5 parts of n-butyllithium. The preparation raw materials of the atomization terminator include 75-85 parts of isopropyl alcohol, 15-20 parts of an antioxidant 1520, 0.5-1.5 parts of cyclohexane, 0.3-0.6 parts of citric acid, 2-4 parts of a plant polyphenol extract and 0.2-0.5 parts of a crosslinking agent. By compounding the antioxidant 1520 and the multi-source purified plant polyphenol extract in the atomization terminator and matching the tannin acid-boric acid composite crosslinking system, a multiple synergistic heat-resistant protection and structure reinforcing mechanism is formed, and the defects of easy oxidative degradation, easy molecular chain rupture and serious performance attenuation of the traditional solution polymerization styrene-butadiene SSBR rubber under a high-temperature environment are effectively improved.

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 invention relates to a preparation method of (bis (trimethylsilyl) amino) tris (pyrrolidinyl) hafnium, which comprises the following steps: (1) reacting bis (trimethylsilyl) sodium amide with hafnium tetrachloride to obtain (bis (trimethylsilyl) amino) hafnium trichloride; (2) reacting tetrahydropyrrole with sodium hydride to obtain sodium pyrrolidinyl; and (3) carrying out a reaction on the (bis (trimethylsilyl) amino) hafnium trichloride obtained in the step (1) and the sodium pyrrolidinyl obtained in the step (2) to obtain the (bis (trimethylsilyl) amino) tris (pyrrolidinyl) hafnium. By optimizing the preparation method of (bis (trimethylsilyl) amino) tri (pyrrolidinyl) hafnium in the prior art, the obtained method is short in synthesis path and simple in synthesis operation, the use of n-butyllithium is avoided, the danger is reduced, the reaction convenience is improved, the raw material cost is low, the product yield and purity are high, and the method is suitable for industrial production. The industrial large-scale production is facilitated.

The invention relates to a preparation method of aldehyde group functionalized halogen-containing helicene, which comprises the following steps: S1, dissolving terephthalaldehyde and p-halobenzyl cyanide in ethanol, adding sodium ethoxide into the solution for reaction, and washing, filtering and drying a reaction product to obtain a solid A; s2, dissolving the solid A in methylbenzene, then adding iodine and epoxypropane for reaction, and washing, filtering and drying a reaction product to obtain a solid B; s3, dissolving the solid B in dichloromethane, adding n-butyllithium into the dichloromethane, sequentially and slowly adding methanol, water and hydrochloric acid after the color of the solution is changed, extracting an organic filtrate after the reaction is completed, carrying out rotary evaporation on the organic filtrate, washing, filtering and drying to obtain aldehyde group functionalized halogen-containing helicene; the invention provides the aldehyde group functionalized halogen-containing helicene and the preparation method thereof, the method is simple to operate, the reaction is simple and convenient, the expansion is flexible, the aldehyde group is successfully introduced into the compound, the reaction steps are reduced, and the experiment complexity is reduced.

The invention relates to the technical field of argon graded replacement, in particular to an argon graded replacement method for synthesizing n-butyllithium. Comprising the following steps: arranging a gas accommodating cavity between adjacent reaction kettles, and controllably communicating the gas accommodating cavity with a gas outlet of a front-stage reaction kettle and a gas inlet pipeline of a rear-stage reaction kettle through a control valve group; firstly, pretreatment equipment (a branch pipe) of a single kettle is started, argon is introduced, mixed gas in a pipeline blind area is removed, then the argon time sequence and flow of upstream, downstream and midstream gas inlets are controlled, a stable pressure gradient is formed, and the mixed gas in the kettle is directionally pushed to a gas containing cavity; mixed gas in the front-stage gas accommodating cavity is introduced into the rear-stage kettle for repeated replacement and is finally discharged from the tail end; according to the method, blind area purification is enhanced, the replacement efficiency is improved, argon consumption is reduced, inert gas waste is reduced, carbon emission reduction is assisted, and atmospheric pollution prevention and control are assisted.

This invention belongs to the field of polymer materials technology and relates to a method for preparing a self-crosslinkable polysiloxane with adjustable boron content. The invention discloses a method for preparing a self-crosslinkable polysiloxane with adjustable boron content, comprising: S1, filling a reaction flask containing carborane with an inert gas, then adding a reaction solvent and dropwise n-butyllithium to the reaction flask under an ice bath environment, and proceeding with a first reaction after the addition is complete; S2, at -40 to -100°C, adding chlorosilane dropwise to the above-mentioned reaction flask filled with inert gas and containing the reaction product of step S1, and proceeding with a second reaction after the addition is complete; S3, removing the lithium salt to obtain the monomer of the polyborosilicate; S4, mixing the chlorosilane monomer of the polyborosilicate with an amine compound, adding a reaction solvent, and performing a three-stage heating reaction to obtain the polyborosilicate; S5, dissolving the polyborosilicate in a solvent and reacting it with a catalyst at 60 to 300°C for 2 to 12 hours.

This invention discloses a novel method for preparing and applying quinoline-2-boron ester. A one-pot method is used with a hexane solution of 2-bromoquinoline and n-butyllithium as raw materials, and tetrahydrofuran as solvent. At -70 to -90°C, 2-lithiumquinoline is formed, which is then captured by triisopropyl borate to generate isopropyl-quinoline-2-boron ester lithium salt. Without separation, the formed isopropyl-quinoline-2-boron ester lithium salt is directly reacted with N-phenyldiethanolamine to generate a novel quinoline-2-boron acid N-phenyldiethanolamine ester. The entire reaction process is simple and easy to operate, and the resulting product is easily separated and purified, with a yield of over 80%. The preparation cost is significantly reduced, the experiment has good reproducibility, and it has significant commercial application potential.

The present disclosure is directed, in general, to synthesizing optionally substituted 2-dicyanomethylene-3-cyano-4-methyl-5-phenyl-5-perfluoromethyl-2,5-dihydrofuran comprising (i) reacting tributyl (1-ethoxyvinyl) tin with n-butyllithium at a temperature of between −30° C. and 10° C. to produce a first reaction product; (ii) reacting the first reaction product with 2,2,2-trifuoroacetophenone to produce a second reaction product: (iii) quenching the second reaction product with an acid to produce 3-hydroxy-3-phenyl-4,4,4-trifluoro-2-butanone; and (iv) reacting the 3-hydroxy-3-phenyl-4,4,4-trifluoro-2-butanone with malononitrile in the presence of base to produce 2-dicyanomethylene-3-cyano-4-methyl-5-phenyl-5-perfluoromethyl-2,5-dihydrofuran.

The application relates to a preparation method of a metal complex and belongs to the technical field of chemical synthesis. The preparation method comprises the following steps: S1, under a protective atmosphere, uniformly mixing n-butyllithium, an activating agent and a solvent to obtain a mixed solution; S2, adding an amine compound into the mixed solution in S1 at-30 DEG C to 0 DEG C to obtain a reaction solution; S3, adding metal chloride into the reaction solution in S2 dropwise at-30 DEG C to 0 DEG C, and performing reaction under the condition of heating and reflux; and S4, after the reaction is completed, removing the solvent under reduced pressure, and then performing reduced-pressure distillation or sublimation to obtain the metal complex. According to the preparation method, the activating agent is introduced, n-butyllithium is completely reacted, side reactions are not caused in the subsequent amplification process, and the amplification process can be realized.

According to the preparation method of the tris (dimethylamino) cyclopentadienyl hafnium provided by the invention, the tris (dimethylamino) cyclopentadienyl hafnium is prepared by adopting the method disclosed by the invention, a better yield can be obtained, and a colorless and transparent product with high purity can be obtained. The preparation method comprises the following steps: S1, reacting an n-hexane solution of n-butyllithium with dimethylamine to obtain a lithium dimethylamino emulsion; s2, dropwise adding the lithium dimethylamino emulsion into a suspension containing hafnium tetrachloride, and stirring for reaction; filtering reaction feed liquid obtained by the reaction, performing vacuum concentration on filtrate to obtain concentrate, and sublimating the concentrate at the temperature of between 0.05 and 0.30 torr and the temperature of between 60 and 70 DEG C to obtain tetra (dimethylamino) hafnium; s3, the tetra (dimethylamino) hafnium and cyclopentadiene are subjected to a contact reaction, and a reaction solution is obtained; and carrying out vacuum concentration on the reaction liquid, and then distilling under the conditions that the pressure is less than 0.15 torr and the heating temperature is 70-80 DEG C to obtain the tris (dimethylamino) cyclopentadienyl hafnium.

This invention provides a primary amine-modified solution-polymerized styrene-butadiene rubber (SBR) and its preparation method. The preparation method includes the following steps: in a polymerization system, using n-butyllithium as an initiator and tetrahydrofuran as a polymerization activator, butadiene monomers and styrene monomers are polymerized to obtain active SBR chains; a diisocyanate compound is added to the polymerization system to terminate the polymerization, and isocyanate groups are introduced at the ends of the active SBR chains to obtain a SBR solution; a terminator is added to the SBR solution, and the mixture is stirred, a precipitate is formed, and dried to obtain the primary amine-modified solution-polymerized SBR. The primary amine-modified solution-polymerized SBR prepared by this method exhibits high polarity and strong bonding with silica fillers, promoting the formation of a more stable and structurally complete filler-polymer network, and significantly improving the dynamic properties of the rubber material.

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 invention discloses a synthesis method of (1R, 4aR, 6S, 8aS)-6-(benzyloxy)-5, 5, 8a-trimethyl-2-methylene decahydronaphthalene-1-methanol, and belongs to the technical field of organic synthesis. The method comprises the following steps: carrying out [2, 3]-Wittig rearrangement reaction on a (4aR, 6S, 8aR)-6-(benzyloxy)-2-[[(tributyltin alkyl) methoxyl] methyl]-5, 5, 8a-trimethyl-3, 4, 4a, 5, 6, 7, 8, 8a-octahydronaphthalene compound in a reactor in an inert atmosphere under the action of n-butyllithium, and carrying out subsequent separation and purification after the reaction is finished, so as to obtain the (1R, 4aR, 6S, 8aS)-6-(benzyloxy)-5, 5, 6, 7, 8, 8a-octahydronaphthalene compound. The method comprises the following steps: adding 2, 3, 5, 8, 8a-trimethyl-2-methylene decahydronaphthalene-1-methanol into a The method provided by the invention has the advantages of simple steps, safe operation, non-toxic and easily available raw materials, simple and easy process and small pollution, and accords with the idea of green chemistry.

The invention discloses a method and a system for continuously preparing 2-(methylthio) phenylboronic acid by a microchannel reactor, and belongs to the technical field of synthesis and preparation of 2-(methylthio) phenylboronic acid. According to the technical scheme, the preparation method comprises the following steps: S1, preparing raw materials: respectively dissolving reactants including 2-methylthio bromobenzene, boric acid ester, hydrochloric acid and n-butyllithium into a solvent, and respectively preparing a 2-methylthio bromobenzene solution, a boric acid ester solution, an acid solution and an n-butyllithium solution; s2, micro-channel reaction: respectively conveying the 2-methylthio bromobenzene solution, the n-butyllithium solution, the borate solution and the acid solution prepared in the step S1 into a micro-channel reactor through a flow rate pump, and carrying out the micro-channel reaction on the 2-methylthio bromobenzene solution, the n-butyllithium solution, the borate solution and the acid solution. And S3, separation and purification: carrying out separation and purification on the reaction liquid obtained in S2 to obtain the required product 2-methylthio phenylboronic acid. According to the invention, simultaneous three-step cascade reaction is carried out in the microchannel reactor to synthesize 2-methylthio phenylboronic acid. The reaction efficiency is improved; and the production energy consumption is reduced.

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 Fe-MoS2 nano-enzyme material as well as a preparation method and application thereof, and the preparation method comprises the following steps: adding MoS2 powder into n-butyllithium in an argon environment, strictly sealing, and carrying out water bath ultrasonic treatment at room temperature to ensure that lithium ions are embedded into MoS2 crystals; then cyclohexane is added in an argon environment for centrifugal washing to remove redundant n-butyllithium, deoxygenated water is added for sealing, water bath ultrasonic treatment is conducted again, and after centrifugal purification, MoS2 nanosheet suspension liquid is obtained. The preparation method comprises the following steps: adding a FeCl3 solution into a MoS2 nanosheet suspension, slightly shaking, freeze-drying to obtain a precipitate, finally obtaining an Fe-MoS2 nano-enzyme material through a Joule heat instantaneous high-temperature method, dispersing the obtained Fe-MoS2 nano-enzyme material with ethanol, adding PVP powder, and stirring for 24 hours to obtain the final material. According to the method, Fe < 3 + > is reduced into Fe atoms through a Joule heat instantaneous high-temperature method, the Fe atoms are embedded into the surfaces of the MoS2 nanosheets, and the Fe-MoS2 nano-enzyme material is formed, has peroxidase-like performance and can be applied to hydrogen peroxide detection.

The invention discloses a catalytic synthesis process of an empagliflozin intermediate compound, which comprises the following steps: dissolving a compound I in an organic solution, adding a catalyst, stirring and mixing at low temperature for 1-2 hours, then adding a compound II, reacting at low temperature, monitoring the reaction by HPLC (High Performance Liquid Chromatography), and separating a product after the reaction is finished to obtain a compound III. The preparation method has the beneficial effects that TMPMgCl.LiCl is used for carrying out oriented metallization on para-position of chlorine atoms and meta-position of benzyl to generate an aryl magnesium reagent, and then the aryl magnesium reagent and hydroxyl-protected glucolactone are subjected to nucleophilic addition reaction to obtain an intermediate compound; a huge TMP (2, 2, 6, 6-tetramethylpiperidyl) group ensures that deprotonation only occurs on a specific C-H bond which is accessible in space and strongest in acidity, extremely high regioselectivity is achieved, and compared with traditional strong bases such as n-butyllithium, the regioselectivity of the method is improved; and diastereoselectivity; therefore, the reaction selectivity is high, and the specificity is strong.