73 results about "Hydroboration" patented technology

The invention discloses a catalytic system for preparing amine compounds through nitro reduction and application of the catalytic system. The catalytic system comprises an alkaline aqueous solution, a reducing agent and a catalyst, the alkaline aqueous solution is an alkali metal hydroxide aqueous solution; the reducing agent is alkali metal hydroboron and / or alkaline earth metal hydroboron; the catalyst is copper salt lewis acid and / or other lewis acid; the other Lewis acid is selected from one or a combination of more of cobalt salt, ferric salt, zinc salt, manganese salt and palladium salt. When the catalytic system is used for reducing the aromatic nitro-compound, the using amount of a reducing agent is small, meanwhile, the using amount of an organic solvent is reduced, the reaction yield is high, the reaction is milder, and amplified production of the process is facilitated.

The application discloses a catalyst for isocyanate borohydration reaction and a preparation and application method thereof. When the catalyst is used for catalyzing the borohydration reaction of isocyanate and borane to synthesize borate, the catalyst has high catalytic activity, mild reaction conditions (the reaction can be carried out at room temperature), short reaction time, high product yield (≥99%), and the reaction is simple, controllable, and simple in post-treatment.

The present application relates to a kind of catalyst composition and its application in catalytic preparation optically active secondary alcohol, the catalyst composition includes chiral ionic bridged aryloxyalkane rare earth complex and additive, the additive is selected from one or more of pyrimidine, N,N-dicyclohexylmethylamine, 4,4'-dipyridyl.The above-mentioned catalyst composition can be used for synergistically catalyzing asymmetric borohydration of chalcone and its derivatives with pinacol borane, and show high catalytic activity and high enantioselectivity, product yield is as high as 99%, ee value can reach 84%, provide a reliable new way for the efficient, high selective synthesis of optically active secondary alcohol.

A full continuous-flow preparation method of (+)-biotin, including: subjecting a cyclic anhydride and a chiral biphenyl propylene glycol to asymmetric ring-opening reaction to produce a first intermediate, which undergoes selective reduction with a borohydride and cyclization with an inorganic mineral acid to produce (3aS, 6aR)-lactone; subjecting the (3aS, 6aR)-lactone and a sulfenylating reagent to sulfenylation to produce (3aS, 6aR)-thiolactone, which undergoes Fukuyama coupling with a zinc reagent in the presence of a palladium catalyst and elimination reaction in the presence of an inorganic mineral acid to produce an alkenyl valerate compound; subjecting the alkenyl valerate compound to reduction in the presence of a Pd / C catalyst to produce a valerate ester, which undergoes hydrolysis to produce a valeric acid salt; and subjecting the valeric acid salt to debenzylation in the presence of an inorganic mineral acid to produce the target product (+)-biotin.

The application is a kind of continuous preparation method and application of core-shell type reduced Cu-based catalyst. The method uses membrane dispersion micro-reactor technology, adopts liquid phase chemical reduction method with potassium borohydride-hydrazine hydrate as double reducing agent, continuously prepares reduced Cu-based nanoscale catalyst, does not need high temperature calcination and hydrogen reduction, can be directly used as active catalyst for catalytic reaction, and realizes green and efficient preparation. The catalyst prepared by the application is used in the reaction of preparing N-butyl-2,2,6,6-tetramethyl-4-piperidinamine from 2,2,6,6-tetramethyl-4-piperidinone and n-butylamine through reductive amination, and excellent catalytic activity and stability are shown.

The invention belongs to the technical field of hydrogen storage materials, and particularly relates to a metal borohydride composite material, a preparation method thereof and a hydrogen storage material. The preparation method comprises the following steps: activating the carbon-based carrier by adopting an alkaline substance; performing gas-phase fluorination treatment on the activated carbon-based carrier; the carbon fluoride-based carrier is mixed with a metal source, a boron source and a solvent, a solvothermal reaction is driven by hydrogen, metal borohydride is synthesized in situ on the surface of the carbon fluoride-based carrier, metal atoms in the generated metal borohydride react with F atoms in the carbon fluoride-based carrier to form a metal-F bridging phase, and meanwhile, the metal borohydride generates metal vacancies. The metal affinity of fluorine in the carbon fluoride-based carrier is utilized to induce nucleation loading of the metal borohydride in the synthesis process of the metal borohydride, and meanwhile, an interface chemical reaction is carried out to generate vacancies and bridging phases. Vacancies weaken B-H bonds, the hydrogen absorption and desorption heat / dynamics of the material are improved, and the bridging phase improves the structural stability and hydrogen absorption and desorption cycle performance of the material.

The invention discloses p-toluenesulfonic acid 8-tert-butyl diphenyl silyloxy-7-methyl octyl ester as well as a synthesis method and application thereof, and relates to the technical field of biopesticides. The preparation method comprises the following steps: taking 8-bromocaprylic acid as an initial raw material, and firstly reacting with t-BuOK and 18-crown ether-6; then reacting with pivaloyl chloride to generate acid anhydride, and then carrying out acylation reaction with 4-benzyl oxazolidine-2-ketone; then carrying out diastereoselective methylation; then, NaBH4 reduction is carried out; carrying out hydroxyl protection; then carrying out hydroboration oxidation reaction; and then carrying out TsCl sulfonylation, so as to synthesize the p-toluenesulfonic acid-8-tert-butyl diphenyl silyloxy 7-methyl octyl ester. The optical purity of the (S)-p-toluenesulfonic acid 8-tert-butyl diphenyl silyloxy-7-methyl octyl ester synthesized in the invention reaches 98%, and the optical purity of the (R)-p-toluenesulfonic acid 8-tert-butyl diphenyl silyloxy-7-methyl octyl ester synthesized in the invention also reaches 98%.

The invention discloses a method for synthesizing alpha-alkenyl boron ester by Markov hydroboration of terminal alkyne, which comprises the following steps of: under the protection of inert gas, carrying out hydroboration reaction on a terminal alkyne compound shown as a formula I and pinacolborane which are used as raw materials and an amide oxazoline cobalt complex which is used as a catalyst in an organic solvent under the action of alkali; the alpha-alkenyl boron ester compound as shown in the formula II is prepared. The invention provides the cobalt complex catalyst with high efficiency, high selectivity and high substrate compatibility and the method, the reaction condition is mild, the operation is simple and convenient, the atom economy is high, and the product yield and the selectivity of the product are improved. When the catalyst is used for a gram-level amplification reaction, a crude product can be purified in a recrystallization or distillation manner, so that the purification step is greatly simplified, and the technical problems of difficulty in separation and low yield in a reaction amplification process of synthesizing alpha-alkenyl boron ester by Markov hydroboration of terminal alkyne in the prior art are solved; and the method has a relatively high industrial application value.

The invention belongs to the technical field of preparation of catalytic materials, and provides a high-density defective polyacid-based metal organic framework catalyst for hydroboration, a preparation method and application. According to the catalyst, a metal organic framework with defects is constructed by adopting a mixed ligand strategy, a polyacid cluster is introduced in situ on the basis of the metal organic framework, and through weak interaction between a cluster object and a subject framework, regulation and control of an oxidation state of a metal node and regulation and control of a supporting effect of an expanded pore space are realized at the same time; therefore, the problem of unstable structure caused by high defect content is overcome, the polyacid-based metal organic framework catalyst with high-density defects is successfully constructed, the catalyst solves the problems that the existing hydroboration reaction is high in temperature, the catalyst is difficult to recycle and the like, efficient conversion of the alkyne hydroboration reaction can be realized, and the yield of the alkyne hydroboration reaction is increased. Moreover, the structure is still stable after repeated cyclic utilization and use, and can be expanded to various alkyne substrates.

The invention discloses high-purity lithium borohydride and a preparation method thereof, and belongs to the technical field of inorganic synthesis.The preparation method comprises the steps that firstly, surface coordination activation is conducted on micron-sized lithium hydride through amino silane, and the reaction activity of the micron-sized lithium hydride is remarkably improved; and then, in a uniform ionic liquid organic solvent composite medium, efficiently synthesizing lithium borohydride with a purified borane complex at a mild temperature. For key impurity chloride ions, trimethylchlorosilane is innovatively introduced to carry out targeted precipitation conversion, and effective removal is carried out before crystallization. And finally, directly separating out a high-purity product from a reaction system through a directional crystallization technology. According to the high-purity lithium borohydride and the preparation method thereof disclosed by the invention, high-efficiency preparation of high-purity and low-chloride-ion lithium borohydride under a mild condition is realized, a key reagent can be recycled, and the problems of high energy consumption and insufficient purity in a traditional method are perfectly solved.

The invention discloses a heat-resistant bio-based degradable polyester material and a preparation method of the heat-resistant bio-based degradable polyester material, and belongs to the field of bio-based high polymer materials. Two brand-new bio-based modified compounds are introduced, wherein one compound is diol with a bicyclic structure prepared by reacting bio-based vanillin with epichlorohydrin and carrying out hydroboration-oxidation, and the other compound is binary acid with an imidazole ring generated by hydrogenating bio-based itaconic acid and condensing the hydrogenated bio-based itaconic acid with ethylenediamine. The preparation method comprises the following steps: melting and mixing 1, 4-butanediol, adipic acid and two modified compounds, adding a catalyst and a nucleating agent, carrying out condensation polymerization under a high-temperature vacuum condition, and drying to obtain the polyester material. According to the material, the heat resistance is synergistically improved through the rigidity of a double-ring structure and the polarity of an imidazole ring, and the material is clear in bio-based source, can be completely biodegraded and is suitable for the fields of high-temperature packaging, degradable meal boxes and the like.

The invention relates to a catalytic system based on at least one neodymocene borohydride, a co-catalyst which is a dialkylmagnesium compound of formula RB-Mg-RL, in which RB is a secondary alkyl of formula R2CH and RL is a primary alkyl of formula RCH2, the Rs, identical or different, being alkyls. The catalytic system addresses the objective of improved macrostructure control in a polymerization process of ethylene or a monomer mixture containing ethylene and a 1,3-diene.

The invention belongs to the technical field of organic synthesis, and particularly discloses a synthesis method of isopinopinone, which comprises the following steps: (1) by taking alpha-pinene as a raw material, hydroborating by using a borane tetrahydrofuran complex, and oxidizing the hydroboration product by using a sodium hydroxide solution and hydrogen peroxide to obtain isopinopinol; (2) performing high-temperature dehydrogenation on the isopinopinol by taking Cu / Ni-Al-SBA-15 as a catalyst to obtain a product, namely isopinopinone; the total loading capacity of Cu and Ni in the Cu / Ni-Al-SBA-15 is 9-12%, the molar ratio of Cu to Ni is (8-10): 1, and the molar ratio of Si to Al in the carrier Al-SBA-15 is (9-11): 1. The conversion rate and the yield of the two-step reaction are relatively high, the dehydrogenation catalyst in the second step can be recycled for more than three times through filtration, and compared with a traditional copper-silicon catalyst, the mesoporous weak-acid molecular sieve serving as a carrier can effectively improve the product selectivity. The purity of the isopinopinone obtained through filtration and rectification can reach 99% or above, the cost can be effectively reduced, and industrial production can be achieved.

The invention belongs to the technical field of organic synthesis, and particularly relates to a branched perfluoropolyether phosphate compound, a composition as well as a preparation method and application of the branched perfluoropolyether phosphate compound. According to the invention, perfluoropolyether alcohol is used as a raw material, and is subjected to substitution, hydroboration and other reactions to prepare the branched perfluoropolyether phosphate compound. The obtained compound has a multi-branched perfluoropolyether chain, after curing, the multi-branched perfluoropolyether group is dissociated on the surface of a metal base material to form a compact perfluoropolyether film layer, excellent hydrophobic and oleophobic properties and smoothness can be provided, in addition, the multi-branched perfluoropolyether is also beneficial to faster energy conversion or release when the compound is stressed, and the performance of the compound is improved. Further, the friction resistance of the coating is favorably improved. Lone pair electrons contained in phosphorus and oxygen heteroatoms in a phosphate group at the tail end of a molecule can be subjected to characteristic adsorption with empty orbits of atoms on the surface of a metal base material, meanwhile, hydroxyl at the tail end of the molecule can also be combined with hydroxyl on the surface of the base material to form hydrogen bonds to be firmly combined with the base material, a compact phosphate protective film is formed, and good protection performance is achieved.

The invention discloses a preparation method of a nucleotide monomer, which comprises the following steps: taking methyl-D-ribofuranoside as an initial raw material, and finally realizing the synthesis of a compound monomer as shown in a formula P through the steps of selective protection, selective deprotection, C-C bond construction, acylating chlorination reaction, basic group introduction through glycosylation, deprotection, hydroboration oxidation and ring closing in sequence. By providing a brand new synthesis method, the reaction yield is improved, the cost of the whole synthesis molecule is reduced, the binding affinity of the prepared target nucleoside monomer serving as a reported drug applied to HCV resistance to RNA can be improved so as to further improve nuclease resistance, and the method has great significance for subsequent nucleic acid drug research.

The invention belongs to the technical field of molecular sieve preparation, and provides a boron-doped MFI type hierarchical pore molecular sieve and a preparation method thereof. The preparation method comprises the following steps: mixing an organic template agent solution, a silicon source and a boron source to obtain reaction precursor gel; and sequentially carrying out hydrothermal crystallization and roasting on the reaction precursor gel to obtain the boron-doped MFI type hierarchical pore molecular sieve, the boron source is hydroboron. According to the method, borate released by slow hydrolysis of hydroboron is used as a boron source, hydrogen released in the hydrolysis process is used as a soft template, modulation of the pore channel structure of the molecular sieve is realized, and the molecular sieve with a micro-mesoporous structure is constructed, so that the mass transfer efficiency of the MFI type molecular sieve is improved, and limitation of steric hindrance and diffusion resistance is reduced.

The invention discloses a mono-nickelocene complex containing dithioformate, and the mono-nickelocene complex containing dithioformate has a structure as shown in the following formula: in the formula, substituent groups R are N (C2H5) 2, NH (C6H11) and OC2H5. The invention discloses a preparation method of the mono-nickelocene complex containing dithioformate, which comprises the following steps: dissolving a disulfide ligand and [Ni2 (C5H5) 3] BF4 in dichloromethane and methanol, reacting in an inert atmosphere, and separating and purifying to obtain the mono-nickelocene complex containing dithioformate. The invention discloses application of the mono-metallocene nickel complex containing dithioformate in catalyzing hydroboration reduction of aldehyde compounds to obtain organic boric acid ester compounds. The mono-nickelocene complex containing dithioformate provided by the invention is novel in structure and simple in preparation process, can efficiently and selectively catalyze the hydroboration reduction reaction of an aldehyde compound under mild conditions to prepare an organic borate compound, and has wide application prospects.

The invention relates to the field of synthesis of organic compounds, in particular to a hydroboration reaction method for catalyzing ketone by a rare earth metal complex. The method for catalyzing the hydroboration reaction of the ketone by the rare earth metal complex comprises the following steps: mixing the rare earth metal complex, pinacolborane, the ketone and a solvent in an inert atmosphere, and reacting, the general chemical formula of the rare earth metal complex is RE (OTf) 3, and RE is a rare earth element. According to the method for catalyzing the hydroboration reaction of the ketone by using the trifluoromethanesulfonic acid rare earth metal (RE (OTf) 3), the catalyst is a commercial product and is low in price, simple and convenient to operate, high in reaction activity, wide in substrate range and high in yield.

The invention discloses a synthesis method of a borohydride anion B11H14 <->. According to the synthesis method, hydroboron and halogenated hydrocarbon are taken as raw materials and are fully pyrolyzed in an organic solvent to prepare precursor salt, the precursor salt and quaternary ammonium salt are subjected to an ion exchange reaction, so that inorganic hydroboron is converted into organic quaternary ammonium salt, and then a poor solvent is adopted to achieve the purpose of crystallization and purification. According to the method, B11H14-can be efficiently synthesized, the yield can reach 70% or above, and the purity of B11H14-can reach 99.5% or above after repeated crystallization. The method is suitable for preparing the quaternary ammonium salt compound corresponding to high-purity B11H14-on a hectogram scale.

This invention provides a method for the catalytic hydroboration of nitrile compounds, belonging to the field of nitrile reduction technology. The method uses nitrile compounds as substrates, molybdenum hexacarbonyl as a catalyst, and pinacolborane as a hydrogen source, with the hydroboration reaction occurring at 78-82°C for 7.5-8.5 h. The reaction utilizes molybdenum hexacarbonyl as a catalyst, which is simple and readily available, requiring no complex synthesis. Furthermore, the reaction process does not require the participation of ligands. Using pinacolborane as a hydrogen source eliminates the need for strictly nitrogen-protected experimental conditions, enabling the hydroboration of nitriles. The substrate applicability is broad, applicable not only to aromatic nitriles but also to aliphatic nitriles and even some dinitriles. The reaction process does not require solvents, making it environmentally friendly. The corresponding hydroboration product is obtained directly after the reaction without further purification, and the reaction yield is high, ranging from 84-100%.

The invention provides a preparation method of an aminopyrimidine compound, which comprises the following steps: step 1, pretreating a reducing agent by using a protic reagent, the reducing agent being selected from a hydroboration reagent; 2, reacting the pretreated reducing agent with Lewis acid; and step 3, adding a compound 1 into the reaction product in the step 2, and carrying out reduction reaction on the compound 1 to obtain a compound I. The preparation method provided by the invention has the advantages of low cost, short reaction time, high product purity, high yield and the like, and is suitable for industrial production.

The invention discloses an application of a copper-based heterogeneous catalyst in catalysis of alkyne and B2Pin2 hydroboration reaction, and the copper-based heterogeneous catalyst is prepared by the following steps: under stirring, adding a copper salt-containing N, N-dimethylformamide-absolute ethyl alcohol solution into a pyridine-3, 5-dicarboxylic acid-containing N, N-dimethylformamide-absolute ethyl alcohol solution, uniformly mixing, and carrying out vacuum drying, thereby obtaining the copper-based heterogeneous catalyst. Reacting at 100-150 DEG C, cooling to room temperature after the reaction is completed, and carrying out solid-liquid separation, solid washing and drying to obtain the product, the copper-based heterogeneous catalyst disclosed by the invention is simple in preparation process, good in stability and recyclable, the reaction can be completed only in 5 minutes when the copper-based heterogeneous catalyst is used for catalyzing an alkyne hydroboration reaction, the reaction condition is mild, the product selectivity and the yield are relatively high, and the copper-based heterogeneous catalyst has good substrate universality.

A process for preparing a polyethylene bearing a terminal ketone function or a copolymer of ethylene and a 1,3-diene and optionally a vinylaromatic compound which contains more than 50 mol % of ethylene and bears a terminal ketone function is provided. The process comprises a polymerization reaction of the monomers in the presence of a borohydrido-neodymocene complex and an organomagnesium reagent, followed by a coupling reaction with a compound containing a nitrile function, and then a hydrolysis reaction.

The invention discloses an anethole synthesis method, and relates to the technical field of fine chemical engineering, and the anethole synthesis method comprises the following steps: 1, taking 4-n-propyl anisole as an initial raw material, and oxidizing the reaction by using air under a solvent-free condition to obtain p-methoxypropiophenone; 2, reducing the p-methoxypropiophenone into 1-(4-methoxyphenyl)-1-propanol by taking aluminum isopropoxide as a catalyst and isopropanol as a reducing agent; and 3, by taking concentrated sulfuric acid as a dehydrating agent, removing hydroxyl of the 1-(4-methoxyphenyl)-1-propanol to obtain anethole. The method has the beneficial effects that air is used for oxidation in the first step, no solvent is used, reaction conditions are simple, post-treatment is convenient, and the reaction conversion rate is high; in the second step, Meerwein-Ponndorf-Verley reduction reaction is used for the first time, dangerous processes such as hydrogenation reduction or hydroboration reduction are avoided, reaction conditions are mild, aftertreatment is simple, and the reaction conversion rate is high.

The invention discloses a cobalt boron hydrogen complex with a hexahedron structure and a preparation method and application thereof, and belongs to the technical field of cobalt boron cluster complexes. The molecular formula of the cobalt boron hydrogen complex with the hexahedral structure is C30H47Co3B2. The invention further discloses a preparation method of the cobalt boron hydrogen complex with the hexahedral structure. The preparation method of the cobalt boron hydrogen complex comprises the following step: reacting the diaryl bridged double cobalt metal complex with borane-tetrahydrofuran (BH3THF) to prepare the cobalt boron hydrogen complex with a hexahedron structure. The cobalt boron hydrogen complex with the hexahedral structure is applied to a catalyst for catalytic hydrogenation reaction. The cobalt boron hydride complex with the hexahedral structure is prepared by adopting a borane direct coordination mode, so that the use of a reducing agent metal hydroboron is avoided, and the reaction is milder and more controllable. The cobalt boron hydrogen complex with the hexahedron structure has a good application prospect.

The invention discloses an application of a heterogeneous catalyst in catalysis of alkyne and B2Pin2 hydroboration reaction, and the heterogeneous catalyst is prepared by the following steps: mixing copper salt, pyrazole-3, 5-dicarboxylic acid and an N, N-dimethylformamide-absolute ethyl alcohol mixed solvent, fully stirring until complete dissolution, carrying out solvothermal reaction at 100-150 DEG C, after the reaction is completed, naturally cooling, and carrying out solid-liquid separation to obtain the heterogeneous catalyst. And washing and drying the solid to obtain the product. The heterogeneous catalyst is simple in preparation process, has good stability and recoverability, and is mild in condition, wide in universality and high in product yield when being used for catalyzing an alkyne hydroboration reaction.

The invention discloses a preparation method and application of a foamed phosphorus-doped carbon nitride confinement metal cobalt photo-thermal catalyst, and belongs to the field of photo-thermal catalytic material preparation and hydroboron hydrogen production. According to the preparation method, melamine is treated through a mixed acid solution of hydrochloric acid and phosphoric acid, foamed phosphorus-doped graphite-like phase carbon nitride is obtained in one step by means of self-assembly of a melamine-cyanuric acid supramolecular precursor, then dipping is performed through a cobalt salt solution, Co < 2 + > is subjected to confined adsorption in a foamed carbon nitride structure, and the carbon nitride is prepared. And finally, reducing the foamed phosphorus-doped graphite-like carbon nitride into metal cobalt in situ through NaBH4, so as to prepare the foamed phosphorus-doped graphite-like carbon nitride confinement cobalt photo-thermal catalyst. The foamed structure is beneficial to transmission of reactant molecules, confined cobalt provides more active sites for surface reaction, the forbidden band width of carbon nitride is reduced after phosphorus doping, and the visible light excitation electron transition capability can be enhanced.

A process for producing diborane is provided which includes mixing boron halide with borohydride ionic liquid for providing a liquid reaction mixture, the liquid reaction mixture chemically reacting for producing gaseous diborane. There is also provided a related composition for producing diborane which includes boron halide and borohydride ionic liquid. Solvents are not needed in the mixture or in the composition to produce the diborane.

The application discloses a method for synthesizing deoxy sugar based on nickel catalysis, and the method comprises the following steps: adding methanol under the protection of inert gas in the condition that a sugar compound is in a nickel catalyst, NaI and borohydride exchange resin, and with or without a ligand, and reacting for 3-5 hours at room temperature to obtain a deoxy sugar compound. The method realizes the synthesis of the deoxy sugar through a sugar unit containing a double bond, and realizes the region control of deoxy through the electronic properties and structural characteristics of related sites.