34 results about "Tert-Butyllithium" patented technology

The invention relates to a counter electrode made of two-dimensional metal sulfide and graphene composite materials, a preparation method of the counter electrode and application of the counter electrode in dye sensitization solar cells. Metal sulfide and graphene composites are loaded on a conductive substrate for preparation. The metal sulfide and graphene composites are dissolved in a solution and are deposited to form a film after being filtered, compressed film plating is carried out on the conductive substrate, drying is carried out, and then the obtained counter electrode is cooled to be at a room temperature, wherein the mass ratio of the metal sulfide to graphene is 20:1 to 20, and the mass ratio of sulfide to tert-butyllithium is 1:5 to 50. Binding agents do not need to be added, and accordingly high-temperature impurity removing is not needed, and the appearance and the structure of the materials can be well maintained. Compared with the material of a Pt counter electrode, the materials are richly reserved in nature, and industrial production can be carried out on a large scale. Compared with materials of other counter electrodes, the materials are easy and convenient to prepare and excellent in catalytic performance, and accordingly the two-dimensional metal sulfide and graphene composite materials have wide application prospects in the field of the dye sensitization solar cells.

The invention relates to a catalyst for preparing n-Butyl butyrate by n-butanal and a preparation method thereof. The catalyst is prepared by the following steps: using a hydroxy-enriched porous organic polymer as a substrate, and forming a complexation structure of Ru on the surface of the substrate; firstly preparing a hydroxy-enriched porous organic polymer material POP; adding tert-butyl lithium or n-butyl lithium, and preparing a polymer POP-Li; and adding ruthenium salt to obtain a polymer POP-Ru. The catalyst has the characteristics of good stability, repeated use, and higher reaction conversion rate and selectivity. The preparation method is capable of creatively fixing Ru ions on the surface of the catalyst, a new idea is provided for the preparation of the catalyst, and the catalyst has the significant application value.

The present invention provides a method for producing various types of arylbis(perfluoroalkylsulfonyl)methane having a bulky aryl group and an electron-accepting aryl group in which synthesis was conventionally considered to be difficult, at high efficiency; a novel arylbis(perfluoroalkylsulfonyl)methane that can be widely applied to asymmertric catalyst, various types of functional materials and the like; and a metallic salt thereof. In addition, excellent catalysts are also provided. An aryl halomethane is reacted with a sodium trifluoromethane sulfinate, the arylmethyl triflone produced thereby is reacted with a t-BuLi and the like, the lithium salt of the arylmethyl triflone obtained is reacted with a trifluoromethane sulfonic acid anhydride, and an arylbis (trifluoromethylsulfony)methane such as pentafluorophenylbis(triflyl)methane, {4-(pentafluorophenyl)-2,3,5,6-tetrafluorophenyl}bis(triflyl)methane and the like are obtained at a high yield.

The invention relates to the field of materials, and particularly discloses metal-phase molybdenum disulfide, an electrode, a preparation method, an electrocatalyst and an energy storage element. Themetal-phase molybdenum disulfide comprises the following raw materials: a molybdenum source, a sulfur source, an organic acid and a proper amount of water; wherein the organic acid is selected from acetic acid or propionic acid. According to the metal-phase molybdenum disulfide provided by the embodiment of the invention, the organic acid is used as an additive to promote the formation of the metal-phase molybdenum disulfide; the content of the metal-phase molybdenum disulfide in the product can reach 72%. The method has the advantages of being simple, safe and suitable for large-scale production, and the problems that existing synthesis of the metal-phase molybdenum disulfide mostly adopts tert-butyl lithium as a raw material, equipment is complex, safety is low, and the production periodis long are solved. The preparation method provided by the embodiment of the invention is low in required reaction temperature, short in reaction time, simple in equipment, energy-saving, safe in used medicines and suitable for large-scale production.

The invention discloses a preparation method and application of an intermediate for preparing fluocalcitol, and belongs to the field of organic chemistry. The preparation method comprises the following steps: by taking a compound 1 as an initial raw material, carrying out addition reaction, tertiary hydroxyl protection, ester group reduction and iodination on the compound 1 and a compound 2 to obtain a compound 6, reacting the compound 6 with triphenylphosphine to form a quaternary phosphonium salt, carrying out Wittg reaction on the quaternary phosphonium salt and a compound 8 to obtain an olefin compound 9, reducing, removing a silyl ether protection group and oxidizing to obtain an intermediate 12; the raw materials are cheap and easy to obtain, the reaction steps are simplified, the preparation cost is reduced, the yield is high, and the product quality is easy to control; use of dangerous samples such as tert-butyl lithium, sodium amalgam, tri-n-butyl hydrogen stannate and carbondisulfide is avoided, the preparation risk is reduced, and large-scale preparation is easy.

This invention is a high-effective high-steroselectivity synthetic method for multi-substituted 3-cyclopentene-1-ketone. It is incldues the following steps: firstly, the derivative of 1,4-diiodo-1,3-butadiene dissolved in the solvent of ethyl ether or tetrachlorofuran reacts with n-butyl lithium or tert-butyl lithium under low temp., CO is further introduced,l quenching reaction is conducted, andthe pure product is obtained further through extracting, stripping, drying, concentrating and decontaminating. The said invented method is scientific and rational, is a most direct and most simple method, and the yield is high, and the product is easily decontaminated.

The invention discloses a rosuvastatin intermediate (R)-tert butyl dimethyl siloxy-glutaric acid monoester preparation method, which belongs to the field of medicine. The method is as follows: compound (S)-4-halogen-3-hydroxy butyric acid ethyl ester is taken as a raw material for ester exchange to obtain other (S)-4-halogen-3-hydroxy butyric ester, (S)-4-halogen-3-tert butyl dimethyl siloxy benzyl butyrate is obtained by protection of the (S)-4-halogen-3-hydroxy butyric ester, and by condensation of the (S)-4-halogen-3-tert butyl dimethyl siloxy benzyl butyrate and chloroformate in the presence of magnesium, tert butyl lithium and n-butyl lithium, (R)-tert butyl dimethyl siloxy-glutaric acid ester benzyl ester is obtained, and the (R)-tert butyl dimethyl siloxy-glutaric acid monoester is obtained by catalytic hydrogenation deprotection. Compared with the original process, the raw material of the process is chiral, natural, needs no resolution and induction and no enzyme hydrolysis to produce the chiral center, so that the product chirality is better. Compared with the original process, enzymes are already-industrialized enzymes, the raw material is easily obtained, reaction conditions are relatively mild, and the process is easy to industrialize. Compared with the original process, the process is shorter and less in three wastes.

The invention discloses a preparation method of a tert-butyllithium solution, which comprises the following steps: (1) in an inert gas protective atmosphere, adding sodium-lithium alloy into an inert solvent, heating while stirring to disperse the sodium-lithium alloy, cooling, and removing the inert solvent to obtain a sodium-lithium alloy dispersion; and (2) in an inert gas protective atmosphere, adding pentane into the sodium-lithium alloy dispersion obtained in the step (1), dropwisely adding a chlorinated n-butane-chlorinated tert-butyl alkane mixed solution at 30-38 DEG C while stirring to carry out reaction, and after the reaction is complete, treating to obtain the tert-butyllithium solution. By adding the catalytic amount of chlorinated n-butane into chlorinated tert-butyl alkane, the reaction for preparing the tert-butyllithium can be initiated and carried out smoothly, thereby implementing industrialized-scale production of the tert-butyllithium.

The invention discloses a dinaphthosilole organic photoelectric functional material. The functional material is synthesized mainly through the following steps: synthesizing a zirconium heterocycle performing water-free and oxygen-free reaction on bis-substituted internal alkyne under the catalytic action of a metallocene zirconium complex; under the catalytic action of cuprous chloride, reacting with tetraiodo-benzene to generate diiodo-naphthalene; synthesizing a dinaphthalene under the lithiation action of n-butyllithium; and finally synthesizing the dinaphthosilole photoelectric material under the lithiation action of tert-butyllithium. In the synthesis process, the method for preparing the diiodo-naphthalene through coupling reaction of heterocyclopentadiene and polyarylated iodide is simple and high in yield; through the activation action of the n-butyllithium, the dinaphthalene can be synthesized from the bimolecular diiodo-naphthalene; and the metallocene zirconium complex is used as a homogeneous olefin polymerization catalyst, so that the catalytic activity and the olefin polymerization stereoselectivity are high. The synthesized dinaphthosilole is of great use in the fields of conductive high-polymer materials, liquid crystal materials and biological active substances.

The invention provides a reaction system for safely adding tert-butyllithium into a reactor. The reaction system comprises a reaction device, a cooling device, a gas protection device and an injector. The reaction device comprises a reaction bottle, a stirring paddle tightly connected to an opening in the middle of the reaction bottle in a sleeved mode and a motor arranged at the upper end of the stirring paddle; the cooling device is arranged under the reaction bottle; the gas protection device is connected with an opening in the right side of the reaction bottle through a three-way valve; the injector comprises a syringe needle, a piston and a needle cylinder, the syringe needle is inserted into a rubber plug to be connected with an opening in the left side of the reaction bottle, the piston is connected with an air cylinder, a cooling layer is arranged on the periphery of the needle cylinder, a reinforcing device is arranged on the periphery of the joint of the syringe needle and the needle cylinder, and a fastening device is arranged on the periphery of the joint of the rubber plug and the opening in the left side of the reaction bottle. The reaction system has the advantages of being simple in structure, reasonable in design, high in automation degree, capable of saving time and labor, safe and convenient in sampling, good in sealing effect and wide in application and has the wide application range.

The invention relates to a synthetic method for 1,4-dithioalkyl benzene and halide thereof. According to the method, 4-bromothiophenol is used as a raw material and reacts with alkyl bromide to synthesize 4-bromo-1-thioalkyl benzene, and then a reaction is carried out to synthesize 1,4-dithioalkyl benzene; or 4-bromothiophenol successively reacts with n-butyl lithium, sulfur powder and acid to synthesize 1,4-benzenedithiol, and then1,4-benzenedithiol reacts with alkyl bromide to synthesize 1,4-dithioalkyl benzene; and 1,4-dithioalkyl benzene can be further halogenated. The synthetic method provided by the invention does not need flammable and combustible t-butyl lithium, so the synthetic method has better security and controllability, is favorable for large-scale industrial production, reduces production cost and is environment friendly.

The invention discloses a dangerous liquid metering system and a metering and conveying method. The dangerous liquid metering system comprises a metering container, a protection fluid storage tank and a fluid metering and conveying device, wherein the top part of the metering container is provided with a protection fluid inlet and an overflow outlet; an overflow valve is arranged at the overflow outlet; the fluid metering and conveying device is used for metering and conveying dangerous liquid or protection fluid; the bottom part of the metering container is provided with a dangerous liquid outlet, and the exterior of the metering container is provided with a heating system for heating the metering container. The dangerous liquid metering system has the advantages that the dangerous liquid can be metered and conveyed; under the condition of avoiding the dangerous liquid touching air, the high-accuracy metering and conveying can be realized; the system can be widely applied to the fields of analysis and synthesis of yellow phosphor, tert-butyllithium, and other highly flammable matters, and the like.

The invention discloses a method for detecting components of mixed gas in a wastewater pool, which comprises the following steps: firstly, mixing 6-methoxy-2-methylquinoline and iodomethane, and performing heating for reaction to obtain faint yellow solid powder; dissolving 7-diethylamino-2-oxo-2H-benzopyran-3-formaldehyde and the product of the faint yellow solid powder prepared in the step 1, stirring and refluxing the mixture, performing cooling to the room temperature, performing filtering, collecting filtrate, performing reduced-pressure spin-drying, and performing silica gel column chromatography separation to obtain an orange solid powder SO2 probe; adding 3, 7-didimethylamino-5, 5-dimethyl diphenyl and tetrahydrofuran, performing cooling, dropwise adding tert-butyl lithium, performing stirring, and performing staying overnight; adding an HCl solution into the mixed solution, performing treating, dissolving residues in trifluoroacetic acid, and performing stirring overnight; continuously alkalifying, extracting, drying and evaporating the obtained solution; and purifying the residue by column chromatography to obtain the dark blue solid NO probe. By adopting a fluorescence analysis technology, the content of the mixed gas in the wastewater pool is easily detected, the response time is short, the sensitivity is high, and the detection range is wide.

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of 2, 5-disubstituted-1, 4-terephthalaldehyde The 2, 5-disubstituted-1, 4-terephthalaldehyde disclosed by the invention is prepared by carrying out oxidation reaction on 2, 5-disubstituted-1, 4-dibromobenzene and DMF under the catalytic action of hexamethylphosphoramide (HMPA) and tert-butyl lithium. According to the method, tert-butyl lithium is added into a reaction system, so that the reaction activity is greatly improved, the reaction yield is greatly improved and is 78% or above under the combined action of tert-butyl lithium and HMPA by virtue of a trace amount of HMPA and the existence form of stabilized carbocations, and the product quantification efficiency is greatly improved.

The invention discloses a benzene ring-containing compound as well as a preparation method and application thereof. The structure of the benzene ring-containing compound provided by the invention is shown as a formula I; wherein R1, R2, R3 and R4 are independently a C1-6 alkyl group, a C3-6 cycloalkyl group or a C6-20 aryl group; and R5 is hydrogen, halogen, C1-C4 alkyl,-COOMe,-COOEt or carboxyl. According to the compound containing the benzene ring, the carbon rhodamine compound can be obtained under the mild condition, strong oxidants such as potassium permanganate and perchlorate do not need to be used, and the use and storage problems of dangerous chemicals such as tert-butyllithium are not involved.

The invention provides a method for preparing 2,4,5- trifluoro-3-methyl benzoic acid. The method is characterized in that 2,4,5-trifluorobenzoic acid reacts with mixed alkali under the condition of an organic solvent so as to obtain metal salt, of which the carboxylic group and the C3 site are substituted; mixed alkali comprises one of n-butyllithium or tert-butyllithium or lithium isopropoxide, one of potassium tert-butoxide or sodium methylate or potassium methoxide and one of 2,2,6,6-tetramethyl-piperidine or diisopropylamine or tetramethyl ethylenediamine or 2-hydrosulfuryl benzothiazole in a mixing manner, and organic solvent is alcohol ether solvent; metal salt reacts with methylating agents, and a substitution reaction is performed at the benzene ring C3 site so as to obtain 2,4,5- trifluoro-3-methyl benzoic acid; and the reaction temperature ranges from subzero 80 to 20 DEG C. The method has the advantages of high reaction temperature and low cost, and is easy for industrialized production.

The invention discloses a preparation method of a microscale single-crystal ternary positive electrode material. The preparation method comprises the steps of sanding and mixing raw materials; grinding nickel carbonyl, cobalt carbonyl, manganese carbonyl and tert-butyllithium in a grinding machine at a high speed according to a mole ratio being (0.2-0.6):(0.2-0.4):(0.2-0.5):(0.95-1.15), wherein the linear speed a of the grinding machine during working is equal to 20-35m/s, a grinding medium is tungsten particle, the particle size b is equal to 0.1-5 millimeter, and the grinding time is b*600/ahours; and sintering a material, in which the material is sintered in an air atmosphere by a conventional round disc electric furnace to obtain the microscale single-crystal ternary positive electrode material, wherein the electric furnace power P is 1,500-3,000W, the electric furnace wire length L is 5-15 meters, and the sintering time is P*0.3/L hours. The microscale single-crystal ternary positive electrode material synthesized by the process has the advantages of low specific area, concentrated grain distributed, high thermal stability and the like; and moreover, since the microscale single-crystal ternary positive electrode material has relatively low specific surface area, the contact degree of the material and an electrolyte is relatively low, and the cycle lifetime of the materialis greatly prolonged compared with a conventional spherical agglomeration material.