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Method for preparing pinacol borane (variants). RU patent 2265023. |
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FIELD: chemical technology. SUBSTANCE: invention relates to technology for preparing organoboron compounds, in particular, pinacol borane (4,4,5,5-tetramethyl-1,3,2-dioxaborolane) representing a monofunctional hydride-borating agent for alkenes and alkynes and for Suzuki's cross-coupling reaction also. Method is carried out by interaction of pinacol (2,2,3,3-tetramethylethylene glycol, 2,3-dimethyl, 2,3-butanediol) with borane reagent in the presence of a solvent and the following isolation of the end product. Gaseous diborane is used as a borane reagent and the process is carried out in diethyl ether medium at range of temperatures 5-36°C, and the process is carried out in the mole ratio of reagents pinacol : diborane = 1:(0.45-0.55), respectively; or the method is carried out by interaction of pinacol with borane reagent and the following isolation of the end product wherein gaseous diborane is used as a borane reagent, and the process is carried out in pinacol melt at temperature ranges 40-80°C. The process is carried in the mole ratio of reagents pinacol : diborane = 1:(0.45-0.55), respectively. Method provides preparing pinacol borane with high yield 90-95% and high purity 99.5-99.8%. Method shows technological simplicity and economy profit in realization in the industrial scale. EFFECT: improved preparing method. 3 cl, 4 ex
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Method for preparing 9-borabicyclo[3,3,1]nonane / 2265022 Invention relates to technology for preparing organoboron compounds, in particular, to the improved method for preparing 9-borabicyclo[3.3.1]nonane. Method for preparing 9-borabicyclo[3.3.1]nonane is carried out by interaction of diborane with 1,5-cyclooctadiene in 1,4-dioxane medium at simultaneous feeding diborane and 1,5-cyclooctadiene at the rate necessary for maintaining the molar ratio 1,5-cyclooctadiene : diborane = (1.9-2.04):1.0, respectively, during all through reaction. The process is carried out in the volume ratio 1,4-dioxane : 1,5-cyclooctadiene = (2.2-4.0):1.0 and at temperature 11-25°C. In preparing 9-borabicyclo[3.3.1]nonane the reaction mass is kept at temperature 65-102°C. The invention provides simplifying technology in preparing 9-borabicyclo[3.3.1]nonane due to exclusion the preliminary preparing borane complex and additional recrystallization of 9-borabicyclo[3.3.1]nonane, enhancing yield of the end product up to 91.0-93.5% of the high quality (the content of basic substance is 99.1-99.9%, melting point is 152-156°C), and possibility for creating the wasteless manufacturing. Method for preparing 9-borabicyclo[3.3.1]nonane shows technological simplicity in its realization and economy profit in its realization in industrial scale. |
Trimethylaminoborane preparation method / 2259373 Invention relates to organoboron compounds technology, in particular to aminoboranes and, more specifically, to trimethylaminoborane, which can be used as reducing and hydroboronizing agents as well as in color photography, in magnetic film manufacture, and as fuel additive to decrease amount of deposits in combustion chamber. Method comprises reaction of trimethylamine with gaseous diborane in organic solvent at reduced temperature. Solvent is selected from aliphatic, cycloaliphatic, and aromatic hydrocarbons with melting temperature not higher than -20°C. Reaction is conducted at temperature from -30°C to 0°C, preferably from -15 to -5°C, at trimethylamine-to-solvent volume ratio 1:(1/5-3.5).Proposed method simplifies preparation procedure owing to eliminated laborious solvent removing vacuum distillation stage and stage wherein of aqueous alkali metal hydroxide is introduced to stabilize aminoborane. Yield of desired product, characterized by high purity, achieves 95-98.6%, which is essentially higher than, for example yield (86%) of morpholinoborane regarded as prototype compound in a known process. |
Derivatives of boranocarbonate, method for their preparing and applying, set for preparing carbonyl complexes of transient metals / 2256664 Invention relates to new derivatives of boranocarbonate of the formula (I): wherein X1 means -H; X3 and X2 mean similar or different substitutes that are taken among the group consisting of -H, -NHxRy at x + y = 3, or -R wherein R means substitute that is bound with nitrogen or boron atom through carbon atom, respectively, and represents methyl or ethyl group; Y means group -OH, -OH2, -OR or -NHR wherein R means substitute that is bound with nitrogen or oxygen atom through carbon atom, respectively, and represents methyl or ethyl group; or their salts. Invention provides using prepared compounds as source of carbon monoxide (CO) and as a reducing agent in preparing carbonyl metal complexes in an aqueous solution. Also, invention involves a method for preparing borane carbonate and a method for reducing with using H3BCO as a reducing agent. |
Phosphorus-boron-containing methacrylate as polyvinyl alcohol-base film material combustion inhibitor / 2254327 Invention relates to compounds with the bond C-P, namely to phosphorus-boron-containing methacrylate that can be used as inhibitor of combustion of polyvinyl alcohol-base film materials. Invention describes phosphorus-boron-containing methacrylate of the following formula: wherein n = 4-8. Polyvinyl alcohol films modified with indicated phosphorus-boron-containing methacrylate shows the enhanced refractoriness, rupture strength up to 206 kgf/cm2, water absorption up to 240% and relative elongation up to 12%. |
Organometallic compound suitable as cocatalyst in polymerization of olefins / 2248980 Invention relates to novel organometallic compounds and to olefin polymerization catalytic systems including such organometallic compounds, and also to a method for polymerization of olefins conduct in presence of said catalytic system. Novel organometallic compound is prepared by bringing into contact (i) compound of general formula I: (I), where Ra, Rb, Rc, and Rd, identical or different, represent hydrocarbon groups; and (ii) Lewis acid of general formula MtR13, where Mt represents boron atom and R1, identical or different, are selected from halogen and halogenated C6-C30-aryl groups. |
Method for preparing lithium complex salts for using in chemical current source / 2246499 Invention relates to a method for preparing lithium complexes salts of the general formula (I): wherein each radical R3-R6 means hydrogen atom (H) or halogen atom (F, Cl or Br). Method involves mixing a) 3-, 4-, 5-, 6-substituted phenol of the formula (III): wherein R3-R6 have above given values with chlorosulfonic acid in acceptable solvent to yield compound of the formula (IV): ; b) intermediate product of the formula (IV) from the stage a) wherein R3-R6 have values given above is subjected for interaction with chlorotrimethylsilane to yield compound of the formula (II) given in the invention description and obtained product is filtered off and subjected for differential distillation; c) intermediate product (II) from the stage b) is subjected for interaction with tetramethanolate borate lithium (1-) in acceptable solvent and the end product (I) is isolated from it. Invention provides the development of a simple method for synthesis of lithium complex salts. |
Method for preparing lithium complex salts for using in chemical current source / 2246499 Invention relates to a method for preparing lithium complexes salts of the general formula (I): wherein each radical R3-R6 means hydrogen atom (H) or halogen atom (F, Cl or Br). Method involves mixing a) 3-, 4-, 5-, 6-substituted phenol of the formula (III): wherein R3-R6 have above given values with chlorosulfonic acid in acceptable solvent to yield compound of the formula (IV): ; b) intermediate product of the formula (IV) from the stage a) wherein R3-R6 have values given above is subjected for interaction with chlorotrimethylsilane to yield compound of the formula (II) given in the invention description and obtained product is filtered off and subjected for differential distillation; c) intermediate product (II) from the stage b) is subjected for interaction with tetramethanolate borate lithium (1-) in acceptable solvent and the end product (I) is isolated from it. Invention provides the development of a simple method for synthesis of lithium complex salts. |
Organometallic compound suitable as cocatalyst in polymerization of olefins / 2248980 Invention relates to novel organometallic compounds and to olefin polymerization catalytic systems including such organometallic compounds, and also to a method for polymerization of olefins conduct in presence of said catalytic system. Novel organometallic compound is prepared by bringing into contact (i) compound of general formula I: (I), where Ra, Rb, Rc, and Rd, identical or different, represent hydrocarbon groups; and (ii) Lewis acid of general formula MtR13, where Mt represents boron atom and R1, identical or different, are selected from halogen and halogenated C6-C30-aryl groups. |
Phosphorus-boron-containing methacrylate as polyvinyl alcohol-base film material combustion inhibitor / 2254327 Invention relates to compounds with the bond C-P, namely to phosphorus-boron-containing methacrylate that can be used as inhibitor of combustion of polyvinyl alcohol-base film materials. Invention describes phosphorus-boron-containing methacrylate of the following formula: wherein n = 4-8. Polyvinyl alcohol films modified with indicated phosphorus-boron-containing methacrylate shows the enhanced refractoriness, rupture strength up to 206 kgf/cm2, water absorption up to 240% and relative elongation up to 12%. |
Derivatives of boranocarbonate, method for their preparing and applying, set for preparing carbonyl complexes of transient metals / 2256664 Invention relates to new derivatives of boranocarbonate of the formula (I): wherein X1 means -H; X3 and X2 mean similar or different substitutes that are taken among the group consisting of -H, -NHxRy at x + y = 3, or -R wherein R means substitute that is bound with nitrogen or boron atom through carbon atom, respectively, and represents methyl or ethyl group; Y means group -OH, -OH2, -OR or -NHR wherein R means substitute that is bound with nitrogen or oxygen atom through carbon atom, respectively, and represents methyl or ethyl group; or their salts. Invention provides using prepared compounds as source of carbon monoxide (CO) and as a reducing agent in preparing carbonyl metal complexes in an aqueous solution. Also, invention involves a method for preparing borane carbonate and a method for reducing with using H3BCO as a reducing agent. |
Trimethylaminoborane preparation method / 2259373 Invention relates to organoboron compounds technology, in particular to aminoboranes and, more specifically, to trimethylaminoborane, which can be used as reducing and hydroboronizing agents as well as in color photography, in magnetic film manufacture, and as fuel additive to decrease amount of deposits in combustion chamber. Method comprises reaction of trimethylamine with gaseous diborane in organic solvent at reduced temperature. Solvent is selected from aliphatic, cycloaliphatic, and aromatic hydrocarbons with melting temperature not higher than -20°C. Reaction is conducted at temperature from -30°C to 0°C, preferably from -15 to -5°C, at trimethylamine-to-solvent volume ratio 1:(1/5-3.5).Proposed method simplifies preparation procedure owing to eliminated laborious solvent removing vacuum distillation stage and stage wherein of aqueous alkali metal hydroxide is introduced to stabilize aminoborane. Yield of desired product, characterized by high purity, achieves 95-98.6%, which is essentially higher than, for example yield (86%) of morpholinoborane regarded as prototype compound in a known process. |
Method for preparing 9-borabicyclo[3,3,1]nonane / 2265022 Invention relates to technology for preparing organoboron compounds, in particular, to the improved method for preparing 9-borabicyclo[3.3.1]nonane. Method for preparing 9-borabicyclo[3.3.1]nonane is carried out by interaction of diborane with 1,5-cyclooctadiene in 1,4-dioxane medium at simultaneous feeding diborane and 1,5-cyclooctadiene at the rate necessary for maintaining the molar ratio 1,5-cyclooctadiene : diborane = (1.9-2.04):1.0, respectively, during all through reaction. The process is carried out in the volume ratio 1,4-dioxane : 1,5-cyclooctadiene = (2.2-4.0):1.0 and at temperature 11-25°C. In preparing 9-borabicyclo[3.3.1]nonane the reaction mass is kept at temperature 65-102°C. The invention provides simplifying technology in preparing 9-borabicyclo[3.3.1]nonane due to exclusion the preliminary preparing borane complex and additional recrystallization of 9-borabicyclo[3.3.1]nonane, enhancing yield of the end product up to 91.0-93.5% of the high quality (the content of basic substance is 99.1-99.9%, melting point is 152-156°C), and possibility for creating the wasteless manufacturing. Method for preparing 9-borabicyclo[3.3.1]nonane shows technological simplicity in its realization and economy profit in its realization in industrial scale. |
Method for preparing pinacol borane (variants) / 2265023 Invention relates to technology for preparing organoboron compounds, in particular, pinacol borane (4,4,5,5-tetramethyl-1,3,2-dioxaborolane) representing a monofunctional hydride-borating agent for alkenes and alkynes and for Suzuki's cross-coupling reaction also. Method is carried out by interaction of pinacol (2,2,3,3-tetramethylethylene glycol, 2,3-dimethyl, 2,3-butanediol) with borane reagent in the presence of a solvent and the following isolation of the end product. Gaseous diborane is used as a borane reagent and the process is carried out in diethyl ether medium at range of temperatures 5-36°C, and the process is carried out in the mole ratio of reagents pinacol : diborane = 1:(0.45-0.55), respectively; or the method is carried out by interaction of pinacol with borane reagent and the following isolation of the end product wherein gaseous diborane is used as a borane reagent, and the process is carried out in pinacol melt at temperature ranges 40-80°C. The process is carried in the mole ratio of reagents pinacol : diborane = 1:(0.45-0.55), respectively. Method provides preparing pinacol borane with high yield 90-95% and high purity 99.5-99.8%. Method shows technological simplicity and economy profit in realization in the industrial scale. |
Synthesis of atorvastatine and intermediate phenylboronate (variants) / 2269515 Disclosed method for production of [R-(R*,R*)}]-2-(4-fluoriphenyl)-β,δ-dihydroxy-5-(1-methyl)-3-phenyl-4-[(phenylamino)-carbonyl]-1H-heptanoic acid semi-calcium salt (atorvastatin) of formula XII includes reaction of preprepared compound of formula Xa with compound of formula IV in solvent mixture selected from group containing xylene, cyclohexane, methyl-tert-butyl ether, diisopropyl ether, acetonitrile, in presence of catalyst selected from group containing pivalic acid, trifluotomethylsulfonic acid, methanesulfonic acid or p-toluenesulfonic acid to form intermediate of formula XIa , followed by hydrolysis of formula XIa and calcium salt production to form target product of formula XII. Claimed compound represents enzyme hydroxymethylglutaryl-CoA reductase inhibitor, and thereby is useful as hypolipidemic and hypocholesteronemic agents. |
Luminescent semiconductor polymer material and a method for preparation thereof / 2283855 Invention provides luminescent material showing semiconductor properties and being product of complex polymerization in glow discharge, which is formed as a supported polymer layer located either between electrodes or on any of electrodes. Starting pyrromethene complex is difluoroborate complex of 1,3,5,7,8-pentamethyl-2,6-diethylpyrromethene (Pyrromethene 567). Method of preparing luminescent semiconductor polymer material comprises glow-discharge polymerization for 2 to 120 min of Pyrromethene 567 vapors at temperature preferably 250-350°C, pressure 10-1 to 10-2 Pa, and discharge power 0.5-3 W. Resulting luminescent polymer is characterized by thickness preferably 0.001-10 μm, conductivity 1·10-10 to 5·10-10 Ohm-1cm-1 (20°C), luminescence emission maximum in the region of 540-585 nm at band halfwidth 55-75 nm. Polymer is obtained with quantum yield 0.6-0.8 and is designed for creation of film light-emitting devices. |
Dyes based on dipyrromethene boron difluoride with biphotonic absorption and their use / 2296333 Invention relates to bioanalytical methods involving dye-labeled indicators. Bioanalytical method without separation is provided directed to measure analyte obtained from biological liquid or suspension, wherein are used: analyte microparticles as first biospecific reagent; and second biospecific reagent labeled with biphotonic fluorescent dye based on dipyrromethene boron difluoride containing at least one water solubility imparting group selected from ammonium salt and sulfonic or carboxylic acid alkali metal salt and at least one chemically active group selected from carboxylic acid, reactive carboxylic acid ester, carboxylic acid anhydride, maleimide, amine and isothiocyanate. In the method of invention, laser is focused onto reaction suspension and biphotonically excited fluorescence from individual microparticles (randomly flowing or oriented by pressure provided by emission of exciting laser through focal volume of laser beam). |
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