260 results about "Butyllithium" patented technology

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 present invention provides a novel polymorphic form of olopatadine hydrochloride ([(Z)-3-(dimethylamino)propylidene]-6,11-dihydrodibenz[b,e]oxepin-2-acetic acid hydrochloride), a selective histamine H1-receptor antagonist that is used for the treatment of ocular symptoms of seasonal allergic conjunctivitis. The present invention also provides novel methods for producing olopatadine on a large scale, and in a manner that is cost effective, provides a low level of impurities and eliminates the need to use the costly and dangerous base, butyllithium, which is used in prior art reactions for making olopatadine. The present invention further provides novel processes for carrying out a large scale production of 3-dimethylaminopropyltriphenylphosphonium bromide and its corresponding hydrobromide salt, which are employed in the production of olopatadine, and pharmaceutically acceptable salts of olopatadine.

The invention discloses a synthetic method of 4-(2,2-difluoro-1,3-benzodioxole-4-yl)pyrrole-3-nitrile. The method comprises the following steps of: preparing an intermediate 2,2-difluorobenz-1,3-dioxole through reacting catechol with dibromodifluoromethane, and preparing an intermediate 2-cyano-3-(2,2-difluorobenz-1,3-dioxole-4-yl)-2-acrylate. The fludioxonil prepared by the synthetic method provided by the invention has the purity of more than 99.0% and the total yield of more than 45.0%; the synthetic method has the advantages of cheap and easily available raw materials, simple process, high product yield in each step, good purity, low production cost, applicability to batch industrial production and the like.

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 relates to a monoacyl ferrocene Schiff base aminocyclotriphosphazene and a synthesis method thereof. The structural formula of the compound is: the present invention makes the prepared monoacyl ferrocene Schiff base amino cyclotriphosphazene have the advantages of ferrocene group and cyclotriphosphazene matrix at the same time, and shows special performance. It has a wide range of application values ​​in chemistry, medicine, catalyst, lubrication and other fields. Compared with the prior art, the method for introducing the ferrocene group into the cyclotriphosphazene matrix of the present invention avoids highly active reagents such as butyllithium, can be operated at normal temperature, and has a simple, safe and low-cost method. features.

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 furanocoumarin-Base derivative, wherein the structural formula of the derivative is as shown in the following formula 6 or 7; the derivative is synthesized by performing ringformation and coupling reaction on parabromoaniline,paraformaldehyde, 4-hydroxycoumarin, isonitrile and n-butyllithium; and the synthesis process is mild in reaction condition, short in reaction timeand high in yield. The Base derivative containing a coumarin fragment has excellent luminescent property and high bioactivity; some of the products have anti-tumor activity, show high-selectivity inhibition on human triple negative breast cancer cells (MDA-MB-231) and have research value of being further developed into anti-tumor medicines; and the other products can be applied to synchronous detection on neuroblastoma metabolites homovanillic acid (HVA) and vanilmandelic acid (VMA) and have the potential of being developed into a high-efficiency fluorescent probe for human neuroblastoma earlywarning and definite diagnosis.

The invention provides a novel pure enantiomer amide type phosphinidene bidentate phosphine ligand with the structural formula shown on the right, wherein, the substituent R on the phosphorus atom of the bidentate phosphine ligand is alkyl or aryl. The synthetic methodsynthesis method is as follows: 4,4',6,6' -quadra (trifluoromethyl) biphenyl -2,2'- diamine is lithiated with n-butyllithium at -40 DEG C to 0 DEG C; then the lithiated 4,4',6,6' -quadra (trifluoromethyl) biphenyl-2,2'-diamine is reacted with dialkyl phosphonium chloride or diaryl phosphonium chloride, and heated naturally to room temperature and reacted for 12-24 hours to get the bidentate phosphine ligand through column chromatography. The invention takes chiral 4,4',6,6'-quadra(trifluoromethyl) - biphenyl -2,2'- diamine and various dialkyl phosphine chlorides or diphenyl(or substituted diphenyl group) phosphine chlorides as raw materials to prepare the amide type phosphinidene bidentate phosphine ligand. The invention enables the pure enantiomer amide type phosphinidene bidentate phosphine ligand to be applied to Rh-catalyzed ene amide and asymmetric hydrogenation of alpha-dehydro amino acid esters and achieves very good results, with the product enantioselectivity up to 99%.

The invention discloses a method for regulating and controlling the structure of an o-carborane derivative through preoccupation. The method comprises the following steps: (1) subjecting o-carborane to lithiation to form a monolithium salt and then reacting the monolithium salt with a CH group protecting agent so as to quantitatively convert the o-carborane into C-H protected carborane; (2) activating C-H by using butyllithium and then carrying out functionalization of a second carbon position; and (3) carrying out deprotection by using tetrabutyl ammonium fluoride. According to the invention, the CH group protecting agent is introduced at first, then the group is subjected to functionalization, and finally deprotection of the group is carried out, so the structure of the o-carborane derivative is regulated and controlled through preoccupation; and thus, a monosubstituted or disubstituted o-carborane derivative is purposefully and selectively synthesized. The obtained monosubstituted or disubstituted o-carborane derivative can be applied to field of aerospace materials like high-temperature-resistant bonding materials and composite materials and has great application prospect in the fields like biological medicines, catalysts, supramolecular systems and high energy fuels.

The invention discloses a synthesis method of pyrotinib, which belongs to the technical field of chemical synthesis of medicines. The preparation method comprises the following steps of firstly, reacting 2-[(4-bromo-2-chlorophenoxy)methyl]pyridine with n-butyllithium at a low temperature, and then carrying out a boronation reaction with an organic boron reagent to obtain [3-chloro-4-(pyridine-2-ylmethoxy)phenyl]boric acid, enabling (2E)-N-(4-amino-3-cyano-7-ethoxy quinoline-6-yl)-3-[(2R)-1-methyl pyrrolidine-2-yl] acrylamide and the obtained [3-chloro-4-(pyridine-2-yl methoxy)phenyl]boric acid to be subjected to a catalytic coupling reaction in a system of a copper catalyst, a base catalyst and a solvent, and acquiring pyrotinib. The method has the characteristics of readily available rawmaterials, simple process, economy, environmental protection and the like, is beneficial to quality control and improvement of final product raw material medicines, is suitable for industrial production and is beneficial to promoting cheap development of the raw material medicines.

The invention belongs to the technical field of medical intermediates, and particularly relates to a synthesis method of (2-fluorin- 6-(trifluoromethyl) pyridine-3-yl) methanol. According to the invention, a compound A is used as an initial raw material and reacts with diisopropylamine under the catalysis of n-butyllithium to obtain a compound B, and the compound B reacts with borane dimethyl sulfide to obtain the (2-fluorine-6-(trifluoromethyl) pyridine-3-yl) methanol, so that the synthesis method of the (2-fluorine-6 (trifluoromethyl) pyridine-3-yl) methanol is provided for the first time. The synthetic method provides a synthetic route for the synthesis of the (2-fluorine-6 (trifluoromethyl) pyridine-3-yl) methanol, and is short in route, reasonable in design, simple to operate and easyto control.

The invention provides a preparation method of a tedizolid phosphate intermediate compound 3-fluoro-4-(6-(2-methyltetrazole-5-yl)pyridine-3-yl)phenyl benzyl carbamate. The method comprises the following steps: carrying out a reaction on 5-bromo-2-(2-methyltetrazole-5-yl)pyridine as a raw material and triisopropyl borate under the action of n-butyllithium to prepare a boric acid intermediate, coupling the boric acid intermediate and 1,2-difluoro-4-nitrobenzene, and finally performing nitro reduction and amidation to obtain the required target product. Compared with the method in the prior art,the preparation method disclosed by the invention has the advantages of easily available raw materials, simple process, economy, environmental protection and suitability for industrial production.

The invention relates to a preparation method of a fluorescent nanoprobe based on a two-dimensional lanthanum metal organic skeleton MOF-La, a prepared probe material and application of the prepared probe in a biosensor. The preparation method comprises the following preparation steps: (1) in an alkali solution, adding 2,2'-thiodiacetic acid or 2,2'-thiodiacetin, La<3+> lanthanum ion inorganic salt, and reacting for 10 to 30 h at the temperature of 120 to 180 DEG C; adding an obtained crystal into an organic solvent, carrying out ultrasonic treatment, performing centrifugation, dispersing into an organic solution of n-butyllithium, and reacting for 15 to 25 h at the temperature of 20 to 30 DEG C under the protection of inert gas, so as to obtain a two-dimensional MOF-La nanomaterial; dispersing the two-dimensional MOF-La nanomaterial in a buffer solution, adding fluorescently-labeled nucleotide chains, and performing centrifugation after reaction at room temperature to obtain the material. The preparation method is simple in preparation conditions, convenient in operation and low in cell toxicity, and the obtained probe has the characteristics of high selectivity and high sensitivity, so that a false positive result is avoided, qualitative performance and quantitative performance are more accurate, and the probe has a good application prospect.

The invention provides a method for preparing 2-methoxy-4-trifluoromethyl-3-pyridinesulfonyl chloride, and belongs to the field of fine chemical engineering. The method comprises the following steps:2-chloro-4-trifluoromethylpyridine used as a starting material is methoxylated to obtain a 2-methoxy-4-trifluoromethyl-3-pyridine compound, the 2-methoxy-4-trifluoromethyl-3-pyridine compound reacts with sulfur powder under the action of butyllithium to prepare a 2-methoxy-3-mercapto-4-trifluoromethyl-3-pyridine compound, and the 2-methoxy-3-mercapto-4-trifluoromethyl-3-pyridine compound is chlorinated and oxidized to obtain the final product 2-methoxy-4-trifluoromethyl-3-pyridinesulfonyl chloride compound. The sulfur powder is used the preparation process of compound III, and thioether compounds are avoided, so odorous odor brought in the production process is eliminated, and environmental pollution is reduced. Hydrogen peroxide is adopted to carry out oxidation, thionyl chloride is adopted to carry out chlorination, and chlorine is avoided, so dangers in the preparation and synthesis process are effectively reduced, and the safety production coefficient is improved.

The invention relates to an integrated rubber SIBR (Styrene Isoprene Butadiene Rubber) and a preparation method thereof. The integrated rubber SIBR is prepared from 10-30 parts by weight of styrene, 20-60 parts by weight of isoprene, 10-30 parts by weight of butadiene, 0.1-1 part by weight of cyclohexane and 0.1-1 part by weight of n-butyllithium. By adopting a method of once charging and reaction extruding, the content of entire alkadiene is increased to above 75 percent; and mechanical properties of tensile strength, bending strength, impact strength, tearing strength and the like of the prepared integrated rubber SIBR are superior to those of an existing product, and important research significance and application value are obtained.

The invention discloses a preparation and application method of a graphene intercalated molybdenum disulfide composite material. The preparation method comprises the following steps: soaking commercial molybdenum disulfide in an n-butyllithium solution, stirring in an argon environment, cleaning, drying to obtain lithium molybdenum sulfide, adding water, and violently reacting to obtain a stripped molybdenum disulfide dispersion liquid A; adding a cationic surface active agent and a single-layer graphene oxide dispersion liquid into the solution A, wherein the molybdenum disulfide layer and the graphene oxide layer are mutually adsorbed; adding a reducing agent, carrying out hydro-thermal treatment, reducing the graphene oxide into graphene, and embedding the graphene into molybdenum disulfide layers; and washing and freeze-drying to obtain the graphene intercalated molybdenum disulfide composite material. The method has the advantages that repeatability is good, and reaction conditions are easy to control. The obtained material is a micron flower assembled by composite nanosheets with a sandwich structure, wherein the thickness of the nanosheets is 10-20 nm, the interlayer spacing of molybdenum disulfide is expanded to 1.16 nm, the hydrophilicity is good, rapid and stable deintercalation of hydrated zinc ions is facilitated, and the zinc storage capacity, the rate capability and the cycling stability are remarkably improved.

The invention discloses an application of n-butyllithium in catalyzing cyanosilylation reaction of ketone and silane. The n-butyllithium has high catalytic activity, low catalyst dosage and good substrate application range. After n-butyllithium, ketone and silane are mixed, the cyanosilylation reaction is carried out to obtain a cyanohydrin compound. The n-butyllithium reagent disclosed by the invention has the advantages of commercialization, easiness in obtaining, low cost, no need for a solvent, environmental friendliness and the like, has a very good catalytic effect on ketone, and is widein substrate application range. Commercial n-butyllithium is used for efficiently catalyzing the cyanosilylation reaction of ketone by using a relatively low dosage of catalyst.

The invention relates to a synthetic method of 1-methyl 4-pyrazole pinacol ester. The biggest advantage of the invention is that the technology is greatly improved; and the problem that the preparation technology of 1-methyl 4-pyrazole pinacol ester is limited in a laboratory and there is no large-scale production is solved. The technical scheme provided by the invention is as follows: the synthetic method of 1-methyl 4-pyrazole pinacol ester comprises The following steps of: Step 1, performing a reaction between 1-methyl 4-pyrazole and triisopropyl borate under the action of n-butyllithium to obtain an intermediate A; and Step 2, performing a reaction between the intermediate A and pinacol under the action of magnesium sulfate to obtain the target product 1-methyl 4-pyrazole pinacol ester. The obtained 1-methyl 4-pyrazole pinacol ester is an important intermediate commonly-used in pharmaceutical chemistry.

The invention discloses an application of n-butyllithium in catalyzing cyanosilylation reaction of aldehyde and silane. The n-butyllithium has high catalytic activity, low catalyst dosage and good substrate application range, and after n-butyllithium, aldehyde and silane are mixed, cyanosilylation reaction is carried out to obtain a cyanohydrin compound. The n-butyllithium reagent disclosed by theinvention has the advantages of commercialization, easiness in obtaining, low cost, no solvent, environmental friendliness and the like, has a very good catalytic effect on aldehyde, and is wide in substrate application range. Commercial n-butyllithium can efficiently catalyze the cyanosilylation reaction of aldehyde by using a relatively low catalyst dosage.

The invention discloses a method for preparing formyl phenylboronic acid, which comprises the following steps: heating halogenated phenylboronic acid in toluene or heptane under reflux for dewatering to form a tripolymer, mixing the tripolymer with dimethylformamide, dropwisely adding n-butyllithium at low temperature to react by a one-pot process, hydrolyzing with hydrochloric acid, and recrystallizing to obtain the formyl phenylboronic acid. The method is simple to operate, avoids the process of separating the intermediate after formyl protection in the conventional technique, has high universality, can obtain favorable yield for ortho-, meta- and para- formyl phenylboronic acids, and is beneficial to scale-up production.

The invention discloses a preparation method of hydroxyphenylboronic acid, which belongs to the technical field of boric acid synthesis in medical intermediates. The method comprises the following steps: starting from bromophenol, carrying out BOC, trimethylsilyl or benzyl protection, forming a Grignard reagent, reacting with borate, or carrying out one-pot reaction with borate and n-butyllithium,and hydrolyzing to obtain hydroxyphenylboronic acid. According to the invention, cheap and easily available protecting groups are adopted, so that the protecting groups are easy to remove during boronation reaction hydrolysis, industrial amplification is easy to realize, batch production is carried out on the scale of dozens of kilograms, and the process stability is good.

The invention discloses base-Schiff base derivatives. A structural general formula of the base-Schiff base derivatives is as shown in a formula [I] as shown in the specification, and the base-Schiff base derivatives are produced by subjecting raw materials of p-bromoaniline, paraformaldehyde, n-butyllithium, p-aminobenzoic acid, substituted o-phenylenediamine and the like to a condensation reaction. The base-Schiff base derivatives fluoresce, emit blue light, and have obvious aggregation-induced emission and solid-state emission, part of compounds have capability of recognizing Al3+, and two compounds have good effects of inhibiting one or two kinds of triple-negative breast cancer cells and liver caner cells, and have small toxicity to normal cells; and three compounds have certain degrees of effects of inhibiting one or more kinds of non-small cell lung cancer cells, triple-negative breast cancer cells and liver cancer cells.