119 results about "Butyllithium" patented technology

The invention belongs to the technical field of organic synthesis and medicinal chemistry, and discloses a total synthesis method of rhododendron heteroterpenin Rhododaurines A-C. The total synthesis method comprises the following steps: carrying out allyl stereoselective addition on a compound 3 and a compound 5 in a toluene solvent under the conditions of catalysis of n-butyllithium and low temperature of-78 DEG C, and constructing a chiral center to obtain a compound 6; removing a methoxy methyl (MOM) protecting group from the compound 6 under an acidic condition, cyclizing, and reacting to generate rhododaurine C (7); the rhododaurine C (7) is subjected to intramolecular [4 + 2] cycloaddition and oxidation reaction in the illumination and oxygen atmosphere of 300-385 nm, and rhododaurine B (8) and an epoxy epimer epinedodaurine B (9) are obtained; and carrying out protonation and rearrangement on the epidodaurine B (9) by virtue of acid catalysis cyclic ether, so as to generate the rhododaurine A (10). The method can overcome the defects that the content of rhododendron miscellaneous terpenoids Rhododaurines A-C in nature is extremely low, and large-scale extraction is difficult.

The invention discloses a synthesis method of a novel benzosuberone compound, and belongs to the field of organic synthesis. The preparation method comprises the following steps: uniformly stirring methyltriphenylphosphonium bromide in a solvent at room temperature, dropwise adding an n-hexane solution of n-butyllithium in an ice-water bath, stirring a reaction system at room temperature for 30-40 minutes after dropwise adding is completed, then adding an initial raw material phenanthrenequinone 1 in the ice-water bath, transferring the reaction system to 40 DEG C for reaction, and after the reaction is monitored to be complete by a TLC (Thin Layer Chromatography) dot plate, filtering, washing and drying to obtain the phenanthrenequinone 1. And pouring the reaction liquid into a silica gel chromatographic column, and simply filtering by using dichloromethane as an eluent to remove salt and phosphine oxide. And performing rotary evaporation to remove the organic solvent to obtain a crude product, and separating and purifying to obtain a target product 2. The method is short in reaction time and low in reaction cost, provides a practical method for obtaining the seven-membered rigid ring skeleton, and has potential value for synthesis of natural products and bioactive molecules.

The invention relates to the field of biomedical polymer materials, and discloses a preparation method of high-viscosity photo-crosslinking sodium hyaluronate hydrogel, which comprises the following steps: dissolving sodium hyaluronate in deionized water / N, N-dimethylformamide to obtain a sodium hyaluronate solution; mixing the sodium hyaluronate solution and the conjugated diene glycidyl ester / N, N-dimethylformamide solution to obtain a pre-formed sodium hyaluronate glue solution; composite antibacterial microspheres and a photoinitiator are added into the preformed sodium hyaluronate glue solution, a photo-crosslinking reaction is performed, conjugated diene glycidyl ester is prepared from raw materials including n-butyllithium, ethyl acetate, 2, 3-dibromo-1-propylene, vinyl magnesium chloride, sodium hydroxide and glycidol, and the conjugated diene glycidyl ester is prepared from raw materials including sodium hyaluronate, sodium hyaluronate and sodium hyaluronate. According to the preparation method disclosed by the invention, the modification reaction and photo-crosslinking time is shortened through the grafting of conjugated diene glycidyl ester, the viscosity of the hydrogel is greatly improved, and the antibacterial property of the hydrogel is improved through the addition of the composite antibacterial microspheres.

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 device comprises a magnetic flocculation reactor, a centrifugal separator is arranged on one side of the magnetic flocculation reactor, a reaction kettle is arranged on one side of the centrifugal separator, and a spiral cleaning machine is arranged on one side of the reaction kettle, and is characterized in that a first driving motor is arranged at the bottom of the centrifugal separator; a driving fulcrum shaft is installed at the output end of the upper surface of the first driving motor, a drum body is arranged in the middle of one side of the outer surface of the driving fulcrum shaft, a plurality of inner cone layers are installed in the drum body, and outer cone layers are arranged on the top of the outer surface of the driving fulcrum shaft side by side. Through cooperation of the first driving motor, the driving fulcrum shaft, the inner cone layer, the outer cone layer and the hydraulic telescopic rod, the taper of the rotary drum body can be dynamically adjusted according to the viscosity of waste liquid, and the solid-liquid separation efficiency is remarkably improved in combination with the spiral flow guide edges on the inner wall.

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 discloses a novel method for synthesizing a ferrocenyl phosphine ligand compound, which comprises the following steps of: reacting a ferrocene compound serving as a starting material with a Grignard reagent and phosphorus trichloride under the action of tert-butyl lithium to generate a ferrocene phosphine ligand, and synthesizing a ferrocene diphosphine ligand in one step. The method is stable and high in practicability, and a novel method for synthesizing the ferrocene ligand compound is provided.

The invention provides a method for preparing dienogest through a one-pot method, and belongs to the technical field of medicine synthesis. The method comprises the following steps: forming ethyl cyano anions from n-butyllithium and acetonitrile under an ultra-low temperature condition, carrying out addition reaction on a compound in a formula (1), quenching with acid after the reaction is finished, and then directly dropwise adding concentrated hydrochloric acid to carry out deprotection-transposition reaction, so as to prepare a compound in a formula (2); and after the reaction is finished, adding a sodium bicarbonate aqueous solution to carry out elutriation, and carrying out secondary refining on an obtained crude product to obtain a refined dienogest product. The dienogest is prepared through the addition and deprotection-transposition reaction one-pot method, the solvent dosage can be effectively reduced, meanwhile, solid waste is reduced, the process cost is reduced, and green chemical industrial production of the dienogest is achieved.

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.

This invention provides a compound for recognizing chiral amino alcohols, a fluorescent probe, its preparation method, and its application. Naphthol and sodium hydride are weighed and dissolved separately in ultra-dry tetrahydrofuran, mixed, and then reacted with bromomethyl methyl ether. The mixture is extracted with ethyl acetate, and the organic phases are combined to obtain product (R)-1. This product is dissolved in ultra-dry tetrahydrofuran, and n-butyllithium is added. The reaction system changes from colorless to brown, and the reaction is allowed to return to room temperature. Ultra-dry N,N-dimethylformamide solution is then added, and the reaction is quenched by adding saturated ammonium chloride solution under ice-water bath conditions. The product is then extracted with ethyl acetate to obtain product (R)-2. Product (R)-2 is dissolved in a mixed solvent of tetrahydrofuran and anhydrous methanol, and sodium triacetoxyborohydride is added. The product is then extracted with ethyl acetate to obtain reduced product (R)-3. Product (R)-3 is dissolved in a mixed solvent of dichloromethane and anhydrous ethanol, and concentrated hydrochloric acid is added. After the reaction is complete, the reaction is quenched with sodium bicarbonate, and then extracted with dichloromethane to finally obtain compound (R)-4, which recognizes chiral amino alcohols.

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.

The application discloses a method for recovering lactic acid methyl ester by catalytic depolymerization of polylactic acid in one pot. The method comprises the following steps: mixing polylactic acid, amine nitrogen ligand and methanol, dissolving by adding a solvent, and then adding a n-butyllithium solution to carry out a depolymerization reaction; and after the reaction is completed, the solvent is removed by vacuum distillation, and the crude product is dried in vacuum to obtain lactic acid methyl ester product. The application does not need to synthesize a complex organic metal catalyst, the depolymerization condition is mild, and the generation of by-products such as low-molecular-weight oligomers is effectively reduced. Therefore, the application has the advantages of simplifying the catalyst preparation process, improving the depolymerization efficiency, reducing the cost and the like, and is suitable for industrialized recovery and cyclic utilization of polylactic acid.

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 novel method for preparing an intermediate compound of aromatic sesquiterpenes Commiphoranes C-D. The method comprises the following steps: substituting the ortho-position of a compound 1 with iodine through n-butyllithium and diiodoethane to obtain a compound 2; removing methoxyl by using boron tribromide to obtain a compound 3; performing nucleophilic substitution on 3-allyl bromide and potassium carbonate to synthesize a compound 4; carrying out Grignard reaction to obtain a compound 5; oxidizing into a compound 6 through a Dess-Martin oxidizing agent; finally, (CH3Si) 3SiH and triethyl boron are subjected to intramolecular free radical series cyclization, so that synthesis of an aromatic sesquiterpene Commiphoranes C-D intermediate compound is successfully completed, sufficient preparation is made for follow-up total synthesis of the natural product, key intramolecular free radical series cyclization has the capacity of efficiently constructing a polycyclic system, and the synthesis process is simple and convenient. According to the preparation method, the defects of expensive reagents, long 14-step linear synthesis route, low yield and the like in the existing synthesis route are overcome; the popularization potential is high.

The invention discloses a method for synthesizing beta-ketone ester, which comprises the following steps: mixing an organic metal reagent solution and an ester A solution in a first microchannel reactor, reacting I to obtain an enol intermediate, mixing the enol intermediate and an ester B solution in a second microchannel reactor, reacting II, and carrying out acid quenching to obtain the beta-ketone ester, the first micro-channel reactor and the second micro-channel reactor are communicated in sequence; the organic metal reagent is selected from at least two of methyl lithium, n-butyllithium, sec-butyllithium, lithium diisopropylamide, lithium bis (trimethylsilyl) amide, sodium bis (trimethylsilyl) amide, potassium bis (trimethylsilyl) amide and potassium tert-butoxide; a solvent in the organic metal reagent solution is selected from at least one of tetrahydrofuran, normal hexane, cyclohexane and normal heptane.

The invention discloses a ferrocenyl chiral diphosphine ligand and a preparation method of an intermediate of the ferrocenyl chiral diphosphine ligand, and belongs to organic synthesis. The method comprises the following steps: dissolving acetylferrocene and a chiral catalyst in an organic solvent, dropwise adding dimethylamine, after the reaction is finished, purifying to obtain a crude product of N, N-dimethyl-1-ferrocenylethylamine, and splitting and dissociating to obtain (S)-(-)-N, N-dimethyl-1-ferrocenylethylamine. The preparation method comprises the following steps: dissolving 2, 4-dichlorophenoxyacetic acid into an organic solvent, dropwise adding sec-butyllithium under a low-temperature condition, continuing to react, dropwise adding an organic solvent solution of iodine under a low-temperature condition, and continuing to react to obtain an iodinated product; then carrying out Ullmann reaction on the iodinated substance under the catalysis of nickel to obtain a coupling product; and finally, dissolving the coupling intermediate and diphenylphosphine in acetic acid, and continuously reacting to obtain a target product. The preparation method provided by the invention has the advantages of cheap and easily available raw materials, less chiral catalyst dosage, less preparation steps, high product yield and good product quality.

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 relates to the technical field of tert-butyllithium preparation, in particular to a tert-butyllithium preparation method which comprises the following steps: preparing raw materials, dissolving lithium and washing oil, mixing the raw materials to start reaction, dropwise adding a modifier, carrying out heat preservation treatment, cooling, settling and taking clear liquid. According to the method, trace impurities on the surface of lithium are removed in the pretreatment link, the PVP coating can block contact of water, oxygen and lithium in a long-acting mode, lithium is prevented from going bad in the earlier stage of storage and reaction, and meanwhile the compatibility of lithium and organic solvents such as n-pentane is enhanced; the interference of impurities on the reaction can be eliminated in a high-purity state of the chlorinated tert-butane, byproducts such as lithium tert-butoxide are prevented from being generated, the moisture in the system is strictly limited by deep dehydration, a stable anhydrous environment is provided for synthesis of the tert-butyllithium, and the reaction efficiency is guaranteed; the operation of deep dehydration and impurity removal by activated aluminum oxide creates a high-cleanliness solvent system for the reaction, avoids the action of water and polar impurities with tert-butyllithium or reaction intermediates, and prevents product decomposition or impurity generation.

The invention discloses a solid defoamer suitable for ceramic glazing and a preparation method thereof. The solid defoamer comprises the following formula: 10-30 parts of rhamnose, 0.0001-0.05 parts of a DMC bimetallic catalyst, 5-20 parts of polyoxyethylene, 5-40 parts of polyoxypropylene, 0.1-2.5 parts of a hydrogen capping agent, 5-20 parts of polydimethylsiloxane, 5-20 parts of carborane, 1-5 parts of n-butyllithium, 0.0001-0.009 parts of cis-dichlorodiammineplatinum, 3-8 parts of methyldichlorosilane, 0.0001-0.01 parts of ferric chloride, 0.8-4 parts of ammonium chloride, 10-30 parts of bovine bone ash, 6-20 parts of fumed silica, 0.001-3.5 parts of light calcium carbonate, 0.8-3.0 parts of phenoxyethanol, 0.001-0.2 parts of iodopropynyl n-butylcarbamate, and 20-40 parts of water. The present invention utilizes carborane to enhance ceramic properties while avoiding the problem of residue disposal. The dispersion of silicon dioxide and light calcium carbonate ensures uniform dispersion and stable ceramic components. The use of cattle bone ash as a dispersant ensures uniform dispersion and a moist ceramic surface.

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 relates to a preparation method of a carborane derivative, which comprises the following steps: reacting carborane with n-butyllithium in an ether solvent in an inert gas atmosphere, adding an inorganic base and a copper catalyst after the reaction is completed, reacting for a period of time, adding pyridine, stirring for a period of time, filtering, washing, and drying to obtain the carborane derivative. And finally, adding a compound L-R1, and carrying out heating reaction to obtain a derivative in which H on one or two carbons on carborane is substituted by R1. According to the preparation method disclosed by the invention, the complete reaction can be carried out only by one solvent, the operation is obviously simpler, and the cost is lower. More importantly, the method provided by the invention significantly improves the yield of the carborane derivative, and has certain application prospects.

The invention discloses a synthesis method of 3-amino-2-(tert-butyldimethylsilyl) phenyl trifluoromethanesulfonate, which is characterized in that a compound 2-bromo-3-nitrophenol is used as a raw material, and the target compound 3-amino-2-(tert-butyldimethylsilyl) phenyl trifluoromethanesulfonate is obtained through four-step reaction. According to the synthesis method disclosed by the invention, tert-butyllithium which is commonly used in the prior art is not used in key steps, and bis (trimethylsilyl) amino lithium (LiHMDS) is adopted to convert a compound 3, namely, 2-bromo-3-((tert-butyldimethylsilyl) oxy) aniline into a compound 4, namely, 3-amino-2-(tert-butyldimethylsilyl) phenol; the reaction risk is greatly reduced, meanwhile, the reaction effect is remarkably improved, no by-product is generated, post-treatment and purification are simple, and the yield is ideal.

The invention discloses a device and method for recovering lithium salts from n-butyl lithium waste liquid. The device comprises a magnetic flocculation reactor, a centrifugal separator is provided on one side of the magnetic flocculation reactor, a reactor is provided on one side of the centrifugal separator, and a spiral cleaner is provided on one side of the reactor. The device is characterized in that: a No. 1 driving motor is provided at the bottom of the centrifugal separator, a driving support shaft is provided at the output end of the upper surface of the No. 1 driving motor, a drum body is provided in the middle of one side of the outer surface of the driving support shaft, a plurality of inner conical layers are provided inside the drum body, and outer conical layers are provided in parallel at the top of the outer surface of the driving support shaft. The device comprises a centrifugal separator in the device, which cooperates with the No. 1 driving motor, the driving support shaft, the inner conical layers, the outer conical layers and the hydraulic telescopic rod, so that the taper of the drum body can be dynamically adjusted according to the viscosity of the waste liquid, and the solid-liquid separation efficiency is significantly improved in combination with the spiral guide ridges on the inner wall.

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 the technical field of semiconductor material preparation, in particular to a preparation method of a niobium-containing metal organic compound. The method comprises the following steps: S1, adding an n-butyllithium solution into a reactor, cooling, then adding tert-butylamine, heating to room temperature, and stirring for reaction to obtain a first intermediate solution; s2, cooling the first intermediate solution, then adding niobium pentachloride, heating to room temperature, and stirring for reaction to obtain a second intermediate solution; s3, cooling the second intermediate solution, introducing HNR1R2, and stirring for reaction to obtain a product mixed solution; and S4, sequentially carrying out solid-liquid separation and reduced pressure distillation on the product mixed solution to obtain the niobium-containing metal organic compound. The method is simple in step and short in reaction time, meanwhile, non-toxic alkane n-hexane is used, harm to the human body and the environment is reduced, n-hexane can be repeatedly used, no waste is generated, and the method is suitable for industrial large-scale production.

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.