528 results about "N-Butyllithium" patented technology

The invention provides a synthetic method of rosuvastatin calcium, which is characterized in that a compound 6 and branched chain react under the action of 2,2,6,6,-tetramethylpiperidine and n-butyl lithium to generate a compound 7, the reaction temperature is increased to minus 30 DEG C and the aspects such as reaction solvent and reaction reagent are improved so that the total reaction route has the advantages of mild condition, low device requirement and suitability for industrial production. Meanwhile, another improved synthetic route of rosuvastatin calcium comprises the following steps: converting esters into acids, synthesizing esters again, and synthesizing the rosuvastatin calcium. The rosuvastatin calcium purity is as high as 99.8%.

The invention relates to a preparation method for a controllable duplex metal alloy nano particle. The metal alloy nano particles is a Pt/Pd-M alloy nano particle, wherein the M is selected from Ni, Fe, Co, Mn, Pd, Zn, Cu and Mo; during preparation, n-butyllithium is used as a strong reducing agent and oleylamine and tri-n-octylphosphine are used as protective agents to reduce acetylacetone, chlorate or acetate of the Pt/Pd-M (M= Ni, Fe, Co, Mn, Pd, Zn, Cu,Mo) at the same time so as to form the uniform and size-controllable Pt/Pd-M alloy nano particle without a concentration gradient. The preparation method is simple and controllable in preparation technology, and can solve the problem that when precursor reduction potentials of two metals are greatly different, one metal can be reduced in prior, so that the alloy nano particle can not be obtained easily, provides a better and universal synthetic method for the preparation of the duplex metal alloy nano particle, and provides a key precursor for the preparation of a new generation of metal-oxide nano hybridization body catalyst used for selective hydrogenation reaction.

The invention discloses a synthetic method of thiophene-3-ethanol. The method comprises the following steps of: adding a halogenated hydrocarbon solvent and ethylene glycol into a reaction kettle, dropwise adding thionyl chloride and preserving heat for reacting; separating liquid and extracting to obtain an organic phase containing a substance shown in the specifications; adding a ruthenium trichloride aqueous solution and a sodium bicarbonate aqueous solution in the presence of the halogenated hydrocarbon solvent and dropwise adding a sodium hypochlorite aqueous solution; after detecting that a system does not have oxidizing property, performing liquid separation, concentration, devitrification and drying to obtain a substance shown in the specifications, adding an ester solvent and butyl lithium into a reaction kettle, adding a prepared ester solution of tribromothiofuran and a prepared ester solution of the substance, separating the liquid and extracting to obtain a system containing a substance shown in the specifications; and adding a dilute sulfuric acid into the system containing the substance shown in the specifications, concentrating, neutralizing, extracting and concentrating to obtain an end product. The method has the advantages of high reaction purity and yield, stable process condition, easiness for operation and mass production capability; and the thiophene-3-ethanol is prepared from tribromothiofuran by performing low-temperature lithiation, so that the use of epoxy ethane serving as an explosive hazard is avoided, and mass production becomes possible.

The invention discloses a preparation method of a layered molybdenum sulfide nanosheet molecule separating membrane. According to the preparation method, n-butyllithium is taken as an intercalation modular and enters a molybdenum sulfide crystal lattice after long-time stirring; water is added for decomposing n-butyllithium, so that the interlayer distances of a molybdenum sulfide sheet are enlarged; molybdenum sulfide is dispersed into monoatomic layer materials through ultrasonic treatment; redundant impurities are removed through dialysis, and a purified and clean molybdenum sulfide water solution is obtained; the obtained molybdenum sulfide water solution is treated with a vacuum filtration method, and the layered molybdenum sulfide nanosheet molecule separating membrane is obtained; and the thickness of the membrane is adjusted by adjusting the volume of the used molybdenum sulfide water solution. A molecule-selective separation membrane is obtained with a method of stacking the monoatomic layer materials to form the membrane; and the material preparation method is simple, the cost is low, and the obtained membrane has size selective separation performance on different molecules.

The invention discloses a preparation method for a molybdenum disulfide nanosheet with a reactive group-containing surface. The preparation method comprises the following steps: adding one part by weight of molybdenum disulfide, 2-5 parts by weight of n-butyllithium and 10-20 parts by weight of n-hexane into a hydrothermal reaction kettle, heating at 50-150DEG C for 0.5-12 hours, cooling to room temperature, performing centrifugal separation and n-hexane washing for five times, drying at 50DEG C for 12 hours so as to obtain molybdenum disulfide powder with lithium ion intercalation, adding 1 part by weight of molybdenum disulfide powder with lithium ion intercalation, 0.05-10 parts by weight of sulihydryl reagents with reactive groups, and 100-1000 parts by weight of water into a flask for performing ultrasonic treatment for one minute to five hours under 50-100 watt, to obtain molybdenum disulfide nanosheet with the reactive group-containing surface. The method is easily available, mild to react, simple to operate, and small in environmental pollution; the prepared nanosheet can be further functionalized, thus having good application prospects.

The invention discloses a method of preparing a superfine monolayer transition metal compound quantum dot solution. The method comprises the following steps: (a) mixing a n-butyllithium solution with a transition metal compound solution to react to obtain an intermediate product, wherein the transition metal compound has the formula of MX2, M is a transition metal element and X is S or Se or Te; (b) drying the intermediate product to obtain a dried product; (c) adding deionized water into the dried product for ultrasonic reaction to obtain an ultrasonic product; (d) centrifuging the ultrasonic product obtained by the step c to obtain the supernate which is the superfine monolayer transition metal compound quantum dot solution. The solution prepared by the invention is uniform in distribution of particle size, has a monolayer structure, and is simple in process equipment, short in reaction period, good in repeatability and easy for industrial production.

The invention discloses a method for preparing high-vinyl solution styrene butadiene through a high-temperature continuous polymerization process. Butyl lithium is taken as an initiator of anionic polymerization, an alkyl tetrahydrofurfuryl ether is taken as a polarity regulator, and the continuous polymerization process is adopted to synthesize high-vinyl solution butadiene styrene at a polymerization temperature of between 100 and 130 DEG C. The vinyl content can reach more than 30 percent, thereby meeting the practical production requirements. The method has the advantages that the alkyl tetrahydrofurfuryl ether is taken as the anion regulator for the homopolymerization of alkadiene or the copolymerization of alkadiene and other olefins; under the condition of the high-temperature continuous polymerization, higher activity is still maintained so as to effectively regulate the vinyl content in the alkadiene.

The invention relates to a fluorescent blue light guest material and its preparation method and use and especially relates to a triphenyl phosphorus oxide-based thermal excitation delayed fluorescent blue light guest material and its preparation method and use. The triphenyl phosphorus oxide-based thermal excitation delayed fluorescent blue light guest material solves the problem that because of large difference of an electron donor and an acceptor, when the electron donor is increased, guest emission wavelength produces red shift so that stable and efficient blue guest luminescence cannot be realized. The blue light guest material has a structural formula shown in the description. The preparation method comprises 1, preparing PXZPhBr, PXZPhBr, PTZPhBr and DMACPhBr, 2, mixing the products obtained through the step 1 and tetrahydrofuran, adding n-butyllithium and diphenylphosphinous chloride into the mixture, adding hydrogen peroxide into the mixture, carrying out stirring and carrying out chromatography and recrystallization. The triphenyl phosphorus oxide-based thermal excitation delayed fluorescent blue light guest material is used for preparation of a thermal excitation delayed fluorescent electroluminescent device. The material utilizes short-axis modification strategy, effectively keeps a matrix triplet state energy level, has a donor-acceptor (D-A)-type molecular structure and balances carrier injection and transmission. The preparation method belongs to the field of fluorescent material preparation.

The invention discloses a method for preparing cyclopentene/cyclohexene-1-boronic acid pinacol ester. The method comprises the step of carrying out coupling reaction on 1-chlorine-cyclopentene/cyclohexene serving as a raw material in an organic solvent A in the presence of monophosphate ligand and a palladium catalyst based on potassium acetate as alkali so as to prepare the cyclopentene/cyclohexene-1-boronic acid pinacol ester. The method is characterized in that the physicochemical reaction at the n-butyllithium and ultralow temperature condition in the literature is avoided, and the palladium catalyst is adopted for catalyzing, so that the amount of the used catalyst is reduced, and the cyclopentene/cyclohexene-1-boronic acid pinacol ester can be prepared in relatively high yield at the acceptable temperature; the boronizing agent n-butyllithium/isopropoxy boronic acid pinacol ester system is replaced by the boronizing agent palladium catalyst/bis(pinacolato)diboron system, and therefore, the cost of the raw materials is greatly reduced, the reaction condition is relatively easy to realize, amplification is easy, and the technical operation is simpler and more convenient.

The invention discloses a synthesis method of Alectinib. The method comprises the following steps: carrying out a borating reaction between 6-bromo-3,4-dihydro-2-naphthalenone and n-butyl lithium and then an organic boron reagent; carrying out a catalytic coupling reaction between the obtained 3,4,-dihydro-2-naphthalenone-6-boric acid and bromoethane; carrying out a dimethylation reaction between the obtained 6-ethyl-3,4-dihydro-2-naphthalenone and iodomethane; carrying out a bromination reaction between the obtained 1,1-dimethyl-6-ethyl-3,4-dihydro-2-naphthalenone and a bromination reagent; carrying out a substitution reaction between the obtained 1,1-dimethyl-6-ethyl-7-bromo-3,4-dihydro-2-naphthalenone and 4-(4-piperidyl)morpholine; carrying out a cyclization reaction between the obtained 1,1-dimethyl-6-ethyl-7-[4-(morpholine-4-yl)piperidine-1-yl]-3,4-dihydro-2-naphthalenone and 3-cyanophenylhydrazine; and carrying out an oxidation reaction between the obtained 9-ethyl-6,6-dimethyl-8-[4-(morpholine-4-yl)piperidine-1-yl]-6,11-dihydro-5H-benzo[b]carbazole-3-formonitrile and dichlorodicyanobenzoquinone to obtain a finished product of Alectinib. The synthesis method has the advantages of relatively short route, simplified operation and relatively low cost and is a green and environment-friendly method suitable for industrial production.

The synthesis of anticancer medicine Raltitrexed with 2, 5-thienyl diformic acid and diethyl glutamate as initial material and through six reaction steps of monocondensation, rearrangement, N-methylation, e;limination of tert-butoxy carbonyl group, condensation with 6-bromomethyl-2-methyl-4-quinbolone and saponification. The present invention has total yield of 18.1%, higher than that of available synthesis line, less reaction steps, mild condition and simple operation, and is suitable for mass production.

The invention discloses a method for preparing 2R-(2, 5-difluorophenyl) pyrrolidine hydrochloride. The method comprises the following steps: (a) reacting a compound (1) with the N, O-dimethyl hydroxylamine hydrochloride to obtain a compound (2); (b) reacting the 1, 4-difluorobenzene and n-butyllithium for 1-3h at -70 DEG C to -50 DEG C in an organic solvent, adding the compound (2) and reacting at the temperature of -70 DEG C to -50 DEG C to obtain a compound (3); (c) reacting the compound (3), a compound (7) and the Ti(OEt)4 in the organic solvent under refluxing to obtain a compound (4); (d) reacting the compound (4) with the sodium borohydride to obtain a compound (5); (e) reacting the compound (5) with the alkali to obtain a compound (6); and (f) reacting the compound (6) in an organic solvent of hydrogen chloride to obtain the 2R-(2, 5-difluorophenyl) pyrrolidine hydrochloride. By adopting the method provided by the invention, the cost is greatly reduced, the yield is obviously increased and the method is safe with a good application future. The reaction route of the method is as shown in the specification.

The invention relates to a method for synthesizing pentafluorophenol by using microchannel reactors, which has the advantages of high reaction speed, short production cycle, low cost and high product purity. The method comprises the following steps: connecting three microchannel reactors in series, and dissolving pentafluorobromobenzene in an ether solvent to obtain a homogeneous mixed solution; respectively pumping the homogeneous mixed solution and an n-butyllithium n-hexane solution into a reactor I to react, thereby obtaining a reaction solution I; respectively pumping borate and the reaction solution I in a volume flow ratio of 1:(5-15) into a reactor II to react, thereby obtaining a reaction solution II; adding dilute hydrochloric acid into the reaction solution II for neutralization until the pH value is 1-3, standing, carrying out oil-water separation, and obtaining a pentafluorobenzene boric acid solution in the oil phase; pumping a 30 mol% oxydol solution and the pentafluorobenzene boric acid solution in a volume flow ratio of 1:(0.5-5) into a reactor III, and reacting to obtain a pentafluorophenol crude product solution; adding a 10 wt% sodium sulfite solution, removing excessive oxydol, washing with water, drying, and rectifying under vacuum to obtain the pentafluorophenol.

The invention provides an organic field effect transistor material based on an oxa-condensed ring, and a synthetic method and application thereof. The method comprises the following preparation steps of reacting diisopropylamine, tetrahydrofuran, n-butyllithium, thiophene-3-ethyl formate, and trimethylchlorostannane; adding 1,4-dibromo-2,5-dimethoxy, tetrakispalladium and anhydrous tetrahydrofuran for reacting; adding 1-bromine-4-hexyl benzene, the anhydrous tetrahydrofuran and an n-butyllithium solution for reacting; mixing with dichloromethane; adding a boron tribromide solution for reacting; reacting with the tetrahydrofuran, the n-butyllithium, and a trimethylchlorostannane solution; reacting with 4,7-dibromo-5,6-difluoro-2,1,3-diazosulfide, tris(dibenzylideneacetone)dipalladium, tris(o-methylphenyl)phosphorus, and anhydrous toluene to obtain the organic field effect transistor material based on the oxa-condensed ring. The invention provides a series of field effect transistor materials capable of realizing high electronic mobility, small reorganization energy and better solubility through selecting different condensed ring units to polymerize with a receptor unit.

The invention discloses a beta-diketone mono-imide vanadium olefinic polymerization catalyst and the manufacture method and the application of ethylene polymerizing, ethylene and norborene polymerizing, ethylene and alpha-alkene or norborene copolymerization. Under the catalysis of formic acid, beta-diketone compound and aniline or the ramification of aniline taking condensation reaction in methanol solution to gain Schiff base; under the non water and non oxygen condition, the Schiff base taking reaction with butyl lithium to gain negative ion ligand; under the non-water, non oxygen condition, the negative ion ligand taking coordination reaction with VCl3, the beta-ketimine vanadium alkene polymerization catalyst could be gained. The invention could catalyze ethylene polymerization, and the copolymerizing of ethylene and alpha-alkene or norborene.

The invention discloses a method for preparing medium-high vinyl block-free solution-polymerized butylbenzene and a product thereof. The method mainly comprises the following steps of: A, undergoing a polymerization reaction on a vinyl aromatic hydrocarbon and an insufficient reacting dose of conjugated diene; and B, continually reacting the remaining reacting dose of conjugated diene. In a medium-high vinyl block-free solution-polymerized butylbenzene product, the content of a styrol block is zero, and the content of the vinyl is between 25 percent and 60 percent. In the method, n-butyl lithium is taken as an initiator for anionic polymerization, a compound product of alkyl tetrahydrofurfuryl ether and sodium alkyl benzene sulfonate is taken as a structure modifier, the alkyl tetrahydrofurfuryl ether can effectively adjust the content of vinyl in the product, the sodium alkyl benzene sulfonate can always keep high reaction activity, and further tail end functionalization is promoted; and high-temperature continuous polymerization is adopted, so that the produce efficiency of the product can be increased, and the product with wide molecular weight distribution can be produced; and the styrol block in the product is eliminated through stepwise reaction, so that practical requirements on production can be met.

The invention provides a method for synthesizing SGLT2 inhibitor drugs. The method comprises the following steps: (a) reacting a compound (1) with n-butyllithium in an organic solvent for 0.5-2 hours, and then dripping an organic solvent dissolved with a compound (2) to react for 1.5-4 hours to obtain a compound (3); or, in a nitrogen atmosphere, reacting the compound (1) with isopropylmagnesium chloride and lithium chloride in the organic solvent for 0.5-1 hour, and then dripping the organic solvent dissolved with the compound (2) to react for 1.5-4 hours to obtain the compound (3); (b) in the organic solvent, carrying out a reduction reaction on the compound (3) to obtain a compound (4); (c) in the organic solvent, carrying out an acetylation reaction on the compound (4), pyridine and acetic anhydride to obtain a compound (5); and (d) carrying out a hydrolysis reaction on the compound (5) to obtain a compound (6), namely the SGLT2 inhibitor drugs. The method provided by the invention is simple in steps, low in cost, high in yield and is suitable for industrial production. The reaction route is as follows in the specification.

The invention relates to an end capping method composing end amidogen cinnamene/ butadiene copolymer and its preparation stockpile stable modified asphalt method. It belongs to polymer modified asphalt technique field. It uses butyl lithium as the anionic polymerization initiator, and 1, 5-dinirogen bicyclo caproylhydride as the anionic polymerization terminator. It makes omega-amidogen cinnamene/ butadiene/ cinnamene ternary block polymer. It adopts that end function SBS and the asphalt are mixed. This can effectively deduce the emanation degree of the SBS modified asphalt and obviously improve storage stability. It applies in modified asphalt manufacture field.

The invention relates to a new preparation route and a new method for a p-toluenesulfonic acid edoxaban hydrate and intermediates thereof. The new method comprises the steps that a high-reactivity compound 109A4x is prepared; a compound 109C6x is prepared by using a new synthesizing method; new compounds 109E8-01, 109E9x and 109T7-01 are prepared; the p-toluenesulfonic acid edoxaban hydrate is prepared by using the intermediates. By using the new method and the new route, the reaction step of copious cooling is omitted, and dangerous elemental sulfur, high-risk n-butyllithium and high-risk azides are prevented from being used. In a word, by means of the method, the p-toluenesulfonic acid edoxaban hydrate and the key intermediates thereof are more easily and safely prepared at a lower coston an industrialization scale.

The invention relates to an oligothiophene derivative and a preparation method thereof. The preparation method of the oligothiophene derivative mainly comprises the following steps of: dissolving 3TB into dichloromethane, adding NBS (N-bromosuccinimide), stirring and reacting so as to obtain 3TB-3Br; adding EDOT (3,4-ethylenedioxythiophene) and tetrahydrofuran into a three-neck flask, controlling the reaction temperature to be minus 78 DEG C, dropwise adding n-butyllithium, gradually raising to be room temperature after the dropwise adding, and continuously reacting; subsequently decreasing the reaction temperature to be minus 78 DEG C, dropwise adding tributyl stannic chloride, gradually raising to be the room temperature after the dripping, and reacting to obtain an EDOT tin reagent; under the protection of nitrogen, adding methylbenzene into the three-neck flask, further adding the 3TB-3Br and the EDOT tin reagent, carrying out backflow reaction so as to obtain a 3TB-3Br crude product, thus obtaining pure 3TB-3EDOT through separation. As cation (or anion) free radicals generated in electrochemical doping are stable, the oligothiophene derivative can be used as a novel organic electrochromic material.

The invention discloses a non-metallocene catalyst and a preparation method and the application thereof. The general structural formula of the non-metallocene catalyst is as shown in formula I. The preparation method of the catalyst comprises the following steps: (1) pyridine or pyridone formaldehyde containing a substituent and amino phenol or amino thiophenol containing the other substituent are put into organic solvent to have reflux reaction and obtain a ligand; and (2) first the organic solution of the ligand obtained in step (1) reacts with butyl lithium, is added with metal halide to react and obtain the non-metallocene catalyst after reaction. When the non-metallocene catalyst is used for ethylene polymerization, not only dichloromethane with polarity but also non-polar toluene and heptane can be selected as the solvent during the ethylene polymerization process, and higher activity is also achieved during the process; and the polyethylene has high molecular weight, and the weight-average molecular weight is 800,000 to 1 million(Formula I is shown as the accompanying drawing.).

The invention provides arylboronic acid derivatives and a preparation method thereof. The two arylboronic acid derivatives are tri(4,4',4'-triboric acid-phenyl)amino(3BzN-3B) and tri(4,4',4'-triboric acid-phenyl)boron(3BzB-3B), and the molecular structures are as shown in the specification. 3BzN-3B and 3BzB-3B are prepared by firstly, respectively reacting tri(4,4',4'-triboric acid-phenyl)amino and tri(4,4',4'-triboric acid-phenyl)boron with n-butyllithium, secondly, respectively carrying out nucleophilic substitution reaction with boric acid ester, and finally carrying out acidolysis by using diluted hydrochloric acid. The products of the arylboronic acid derivatives, namely, the 3BzN-3B and the 3BzB-3B are expected to be excellent environment-friendly organic fire retardants.

The invention provides a continuous tank reactor and a continuous tank reaction system with n-butyllithium participating in production. The continuous tank reactor comprises N continuous reaction kettles successively connected in series. Each continuous reaction kettle comprises a body, which has a reaction chamber, a feed inlet, an overflow mouth and a discharge port. N is a natural number whichis greater than or equal to 2. The overflow mouth of the N-1 continuous reaction kettle is communicated with the feed inlet of the N continuous reaction kettle. The continuous tank reactor issuitable for chemical reactions with chemical substances having active chemical properties such as n-butyllithium, etc. participating in the reactions. In actual production, an appropriate number of the continuous reaction kettles can be selected according to the need of reacting dose for a continuous reaction. Thus, lots of reaction raw materials transferred at a time or dropwise added for a longtime in single-kettle batch production are reduced, reaction operational risk is reduced, and safety and reaction efficiency are enhanced.