128results about "Preparation by reductive alkylation" patented technology

The invention discloses a nitrogen-containing carbon hollow sphere supported cobalt-based catalyst as well as a preparation method and application thereof, and belongs to the technical field of catalyst preparation. According to the preparation method, ammonia water, tetraethyl orthosilicate, polyoxyethylene polyoxypropylene ether triblock copolymer, resorcinol and a formaldehyde solution are fully reacted in a mixed solvent of deionized water and ethanol by virtue of a template method, and the nitrogen-containing carbon hollow spheres are obtained after calcination and etching; then carrying out surface modification on the nitrogen-containing carbon hollow spheres, and uniformly loading cobalt metal by virtue of the structure guiding effect of hexamethyleneimine and sodium citrate dehydrate; the prepared nitrogen-containing carbon hollow sphere supported cobalt-based catalyst has abundant highly-exposed Co-N-C active sites, has wide substrate universality, has good catalytic activity and selectivity for amination reactions with various long-chain fatty aldehydes, fatty ketones, cyclic fatty ketones, aromatic aldehydes and ketones as raw materials, and can realize efficient catalytic amination reactions of carbonyl compounds.

The present invention relates to a method for continuously preparing 5-amino-1-pentanol, 1-amino-2-pentanol, and 1,5-pentanediamine using furfural as a raw material. The method comprises the following steps: After hydrogen and the raw material liquid are preheated to 20-150 °C in a preheater, they are simultaneously introduced into a fixed-bed reactor equipped with two sections of catalysts, and reacted at 30-150 °C and a reaction pressure of 0.1-8 MPa to obtain 5-amino-1-pentanol, 1-amino-2-pentanol, and 1,5-pentanediamine; the first catalyst is a metal catalyst supported on graphitic carbon nitride; the active metal of the second catalyst is one, two, or more of Ru, Pt, Rh, Cu, Co, and Ni; the carrier of the second catalyst is γ-Al2O3, TiO2, SiO2, ZrO2, CeO2, ZSM-5, cerium-zirconium solid solution, or activated carbon. The present invention solves the problem of poor selectivity in the process of generating 1,5-pentanediamine, and the product distribution can be changed by changing the catalyst.

The invention belongs to the technical field of catalysts, and particularly relates to a catalyst, a preparation method thereof and application of the catalyst in synthesis of primary amine compounds. The preparation method of the catalyst comprises the following steps: dissolving Ni (NO3) 2 and terephthalic acid in a solvent, uniformly mixing, carrying out a hydrothermal reaction at a certain temperature to obtain Ni-MOF, washing, drying, and reducing in an H2 / Ar atmosphere to obtain the catalyst Ov-NiO / Ni-C-T (X) (wherein T represents the reduction temperature, the unit is DEG C, and X represents the reduction time, the unit is h). The preparation method of the catalyst is simple, the catalyst can be recycled for 7 times without obvious loss of catalytic activity and selectivity, and the catalyst has high catalytic activity for synthesis of primary amine through reductive amination of aldehyde compounds and ketone compounds.

The invention discloses preparation and application of a reductive amination catalyst. The preparation method of the catalyst comprises the following steps: step 1, preparing an SrTiO3 carrier; step 2, loading a nickel source into the prepared SrTiO3 carrier to form a nickel-loaded SrTiO3 catalyst precursor; and step 3, roasting the SrTiO3 catalyst precursor to obtain the SrTiO3 loaded nickel catalyst. Large-scale production of the non-noble metal catalyst is realized by adopting a co-precipitation method and an impregnation method which are simple in process and environment-friendly under the condition of room temperature, the obtained material can be used for reductive amination reaction of acetophenone under the condition of taking water as a solvent and shows excellent catalytic performance, and after 50 times of application, the acetophenone conversion rate is gt; the selectivity of alpha-phenylethylamine is gt; the selectivity of the alpha-phenethyl alcohol is 1t; and 2%.

The invention discloses a surfactant for selectively extracting perrhenate and an application method of the surfactant, the surfactant is a high-selectivity diamino surfactant, and ammonium perrhenate can be separated and enriched by the surfactant. The application method comprises the following steps: adjusting the pH value of a perrhenate-containing leachate, sequentially adding the diamino surfactant and the bubble dispersant, and introducing gas for flotation to obtain a rhenium-rich component; and after the rhenium-rich component is subjected to pH adjustment, a stripping agent is added for stripping, so that ammonium perrhenate with relatively high purity is obtained. The method is simple in technological process, low in operation cost, good in selective separation effect on ammonium perrhenate, capable of effectively overcoming the defects that a traditional solvent extraction process is tedious and high in extraction agent consumption, and suitable for selective separation of ammonium perrhenate under the low-concentration condition.

The present invention provides a method for preparing the active pharmaceutical ingredient of fenfluramine. Aspects of the present invention include (a) hydrolyzing a 2-(3-(trifluoromethyl)phenyl)acetonitrile composition to produce a 2-(3-(trifluoromethyl)phenyl)acetic acid composition; (b) reacting the 2-(3-(trifluoromethyl)phenyl)acetic acid composition with acetic anhydride and a catalyst to prepare a 1-(3-(trifluoromethyl)phenyl)propan-2-one composition; and (c) reducing and aminating the 1-(3-(trifluoromethyl)phenyl)propan-2-one composition with a borohydride reducing agent and ethylamine to produce a fenfluramine composition. The present invention also provides a composition and a pharmaceutical ingredient comprising a pharmaceutically acceptable salt of fenfluramine prepared according to the method and having less than a total of 0.2% by weight of trifluoromethyl regioisomers.

A method for preparing the insecticide N-(1-methylcyclopropyl)-2-(3-pyridinyl)-2H-indazole 4-carboxamide is disclosed. A method for preparing the intermediate N-(1-methylcyclopropyl)-2-(3-pyridinyl)-2H-indazole 4-carboxamide is also disclosed.

A process for the manufacture of ethyleneamines and ethanolamines, comprising the steps of (i) converting a glycolaldehyde derivative of formula (II), in which R2, R3 are—the same or different—hydrogen, alkyl, such as C1-6-alkyl, or cycloalkyl such as Cs-e-cycloalkyl; and an animating agent of formula (III); in which R1 is hydrogen (H), alkyl, such as C1-6-alkyl, or cycloalkyl such as C3-6-cycloalkyl, in the gas or liquid phase; (ii) feeding the reaction products obtained in step (i) into a hydrogenation reactor, where the reaction products are converted with hydrogen in the presence of a hydrogenation catalyst.

The application discloses a supported nanomaterial, a preparation method thereof, and a method for synthesizing 6PPD by using the supported nanomaterial as a catalyst. The preparation method of the supported nanomaterial comprises the following steps: obtaining a mixture containing a nitrogen source, a carbon source and a noble metal source; and performing calcination I, calcination II and acid pickling on the mixture to obtain the supported nanomaterial; the atmosphere of the calcination I and the calcination II is nitrogen; the conditions of the calcination I comprise that the temperature is 555 DEG C to 855 DEG C, and the time is 2h to 6h; the conditions of the calcination II comprise that the temperature is 955 DEG C to 1155 DEG C, and the time is 2h to 4h. The noble metal element is modified on the nitrogen-doped carbon nanosheet by a pyrolysis one-step method. The supported nanomaterial is used as the catalyst for producing 6PPD, and the copper damage problem in the industrial production can be solved, and the ketone to alcohol side reaction phenomenon can be reduced. The catalyst has high activity and high selectivity in the catalytic hydrogenation for preparing 6PPD, and has a good application prospect.

The present invention relates to a process for making secondary and / or tertiary amines comprising an amination step, said amination step being carried out by gas phase reaction of a primary or secondary alcohol and / or ketone with ammonia or a primary or secondary amine in the presence of a catalyst, said catalyst comprising copper and doped with manganese, the amount of manganese being between 1% and 10% by weight relative to the total weight of the catalyst.

A method for preparing the insecticide N-(1-methylcyclopropyl)-2-(3-pyridinyl)-2H-indazole 4-carboxamide is disclosed. A method for preparing the intermediate N-(1-methylcyclopropyl)-2-(3-pyridinyl)-2H-indazole 4-carboxamide is also disclosed.

A process for the purification of pentamethyl diethylenetriamine (PMDETA) comprising one or more by-products selected from the group consisting of N,N,N",N"-tetramethyldiethylenetriamine, N,N,N'-trimethyl-N'-[2-(methylamino)ethyl]ethane-1,2-diamine and N,N,3-trimethyl-1-imidazolidineethanamine, comprising the steps: a) providing a crude PMDETA mixture comprising one or more of the by-products; b) adding a compound reactive with the by-products; c) reacting the by-products with the reactive compound to obtain derivatives of the by-products; d) distillative separation of PMDETA from the by-product derivatives obtained in step c) to obtain pure PMDETA.

The invention discloses a method for preparing primary amine chemicals by hydrogenation amination of aldehyde and ketone through a platinum group monatomic doped nickel-based layered hydroxide catalyst, and belongs to the technical field of heterogeneous catalysis preparation of high-quality chemicals. The method comprises the following steps: by taking aldehyde and ketone chemicals as raw materials and ammonia gas as a gas source, carrying out hydrogenation amination reaction in a reaction solvent under the action of a platinum group monatomic doped nickel-based layered hydroxide catalyst and a hydrogen atmosphere to prepare a primary amine chemical; the platinum group single atom is any one of palladium, platinum, ruthenium, iridium or rhodium; wherein the effective active components on the nickel-based layered hydroxide carrier are composed of nickel metal and other metals, and the other metals are one or more of zinc, magnesium, aluminum, cerium, manganese, zirconium, iron, niobium or copper. The primary amine chemical prepared by the method has very high economic value.

The disclosure is directed to cocrystals of fasoracetam, including R-fasoracetam, and various coformers. Crystalline materials comprising fasoracetam, including R-fasoracetam, are also provided. The disclosure further includes pharmaceutical compositions and methods of treatment of the cocrystals and crystalline materials of the disclosure.

The invention discloses a catalyst for preparing N-(1-ethyl propyl)-3, 4-dimethylaniline through continuous catalytic hydrogenation and a preparation method and application thereof, the catalyst comprises a carrier, and an active component platinum and an auxiliary component which are loaded on the carrier, the auxiliary component is at least one of sodium citrate, disodium ethylene diamine tetraacetate, sodium metavanadate, oxalic acid, zirconium oxychloride, yttrium nitrate or sodium carbonate; and the active component and the auxiliary component both account for 0.1-10% of the mass of the catalyst. The catalyst is used for preparing N-(1-ethyl propyl)-3, 4-dimethylaniline through hydrogenation, the reaction can be continuous, the safety performance is better, and the catalyst has high catalytic activity and stability.

The invention discloses a method for realizing N-methylation of a nitrogen-containing compound through controllable depolymerization of polyformaldehyde and application of the method, and belongs to the technical field of solid waste recycling, the method comprises the following steps: constructing a reaction system comprising polyformaldehyde, the nitrogen-containing compound, a supported metal catalyst and a solvent, carrying out depolymerization upgrading reaction at the temperature of 160-240 DEG C for 0.2-10 hours to realize N-methylation of the nitrogen-containing compound, so as to obtain a corresponding N-methylated derivative of the nitrogen-containing compound; the solvent is an organic solvent or a mixture of the organic solvent and water; the nitrogen-containing compound is an aliphatic amine compound, an aromatic amine compound or an aromatic nitro compound. The method disclosed by the invention is simple in process, the POM-mediated nitrogen-containing compound can be converted into the corresponding N-methylated derivative by a one-pot method, the side reaction is few, the product yield is high, and the method has a wide application prospect in the field of POM waste treatment.

Methods are provided for the synthesis of cannabinoids, including cannabidiol (CBD), cannabinol (CBN), cannabichromene (CBC), cannabidiolic acid (CBDA), cannabigerol (CBG), cannabigerolic acid (CBGA), cannabidivarin (CBDV), cannabidibutol (CBD-C4), dihydrocannabidiol (DCBD), tetrahydrocannabivarin (THCV), analogs thereof, and precursors to the foregoing. One method employs phloroglucinol or a phloroglucinol analog as a starting material. The syntheses are stereospecific, efficient, selective, and cost-effective, with little or no potential for generation of THC ((−)-trans-Δ9-tetrahydro-cannabinol) or any other psychoactive side product. Telescoped syntheses are also provided, as are new cannabinoids, pharmaceutical formulations, and methods of use.

The application discloses a synthesis method of a trident connecting segment which can be used for improving hydrophilicity of an antibody drug conjugate, and relates to the field of organic synthesis. The {[5-amino-2-(3,3,4,4-tetramethyl-2-oxa-3-silapent-1-yl)phenyl]methyl}(methyl)amino)methane acid-2-methylpropan-2-yl ester can be used for connecting a hydrophobic dipeptide, a hydrophilic chain and a small molecule drug in an ADC drug, so as to prolong the action time of the ADC drug. The application takes cheap and easily obtained commercial raw material 2-bromo-5-nitrobenzaldehyde as a starting raw material, and successfully prepares the target product through seven steps of conventional transformation such as reduction amination, protection, coupling, ozonation and nitro reduction, with a total yield of about 60% and a scale of hundreds of grams. The starting raw material is cheap, the operation and treatment are simple, and the reaction condition is mild, so that the application is a brand-new process synthesis route, and has good economic benefits and market prospects.

The invention relates to the technical field of organic synthesis, and particularly discloses a synthesis method of 4, 4 '-methylene bis (N-cyclohexylcyclohexane-1-amine). The method comprises the following steps: mixing cyclohexanone and 2-methylpyridine borane, and heating to a reaction temperature; the preparation method comprises the following steps: reacting 4, 4 '-diaminodicyclohexylmethane with heat preservation, after the reaction is finished, cooling to room temperature, mixing a reaction solution with diluted hydrochloric acid, adding an organic solvent for extraction, collecting a water phase, then adjusting the pH value of the water phase to 8-9, adding an organic solvent for extraction, collecting an organic phase, drying and concentrating to obtain the 4, 4'-methylene bis (N-cyclohexylcyclohexane-1-amine). The synthesis method provided by the invention has the advantages of simple process, no need of high temperature and high pressure, mild and controllable reaction conditions, no influence of water in a reaction system, high conversion rate and good selectivity, conforms to the concept of green and safe production, and has a good development prospect.

The application provides a catalyst, a preparation method thereof and application of the catalyst in preparation of hexanediamine. The preparation method of the catalyst comprises the following steps: step A: performing crystallization treatment on a catalyst precursor to obtain a crystallization system; the catalyst precursor comprises at least one of a titanium-containing SAPO molecular sieve raw material source mixed solution and an alkalized TS-1 molecular sieve catalyst; and step B: performing post-treatment including calcination treatment on the crystallization system to obtain the catalyst. The method can effectively reduce generation of non-framework titanium species, optimize pore structure and active distribution, and thus improve structural stability and anti-inactivation capacity of the catalyst.

The application relates to a preparation method of a novel multi-channel Co / CM ceramic catalytic membrane, and belongs to the technical field of catalytic membrane preparation. The catalytic membrane takes a multi-channel ceramic membrane as a carrier, ZIF-67 is assembled layer by layer on the surface and in the hole of the ceramic membrane, and a one-step pyrolysis reduction method is adopted to prepare the catalytic membrane. The application has the advantages that nanoscale Co particles are loaded on the ceramic membrane to replace noble metals, the surface of the Co particles is wrapped by carbon and nitrogen, the loss of the Co particles in the reaction process is effectively inhibited, the obtained Co / CM ceramic membrane has excellent catalytic activity and stability, the problem of difficult separation of a traditional catalyst from products is solved, and the Co / CM ceramic membrane can be widely applied to a hydrogenation reaction process.

Methods are provided for the synthesis of cannabinoids, including cannabidiol (CBD), cannabinol (CBN), cannabichromene (CBC), cannabidiolic acid (CBDA), cannabigerol (CBG), cannabigerolic acid (CBGA), cannabidivarin (CBDV), cannabidibutol (CBD-C4), dihydrocannabidiol (DCBD), tetrahydrocannabivarin (THCV), analogs thereof, and precursors to the foregoing. One method employs phloroglucinol or a phloroglucinol analog as a starting material. The syntheses are stereospecific, efficient, selective, and cost-effective, with little or no potential for generation of THC ((−)-trans-Δ9-tetrahydro-cannabinol) or any other psychoactive side product. Telescoped syntheses are also provided, as are new cannabinoids, pharmaceutical formulations, and methods of use.

The application discloses a preparation method of butanediamine, which comprises the following steps: synthesizing cyanopropyl aldehyde by adopting synthesis gas and acrylonitrile, and then performing ammoniation hydrogenation on the cyanopropyl aldehyde to produce 1,3-butanediamine and 1,4-butanediamine in a combined manner. According to the synthesis route, the total yield of the product butanediamine is greater than or equal to 95%, and compared with the hydrocyanic acid method, the ammoniation hydrogenation catalyst has the advantages of low single consumption and low total production cost of the product.

Provided is a polyalkyl p-phenylenediamine anti-aging agent having a structure as shown in formula I, and an intermediate thereof and a preparation method therefor. The polyalkyl p-phenylenediamine anti-aging agent has good thermo-oxidative aging resistance and ultraviolet aging resistance.

The present invention discloses an environmentally friendly p-phenylenediamine antioxidant, its preparation method, and application. The environmentally friendly p-phenylenediamine antioxidant has a structure represented by formula (I). The p-phenylenediamine antioxidant with the structure represented by formula (I) exhibits excellent anti-aging properties and does not produce highly toxic quinone products, providing protection against ozone, heat, and oxygen aging. Rubber vulcanizates using the environmentally friendly p-phenylenediamine antioxidant of the present invention exhibit excellent physical properties and aging resistance. Toxicity testing of rubber residues revealed no highly toxic quinone products, demonstrating environmental friendliness and non-toxicity. #imgabs0#

The present application relates to the technical field of pharmaceutical intermediates, and in particular to a synthesis method of chiral indanamine, which comprises the following steps: taking indanone as a raw material, using a chiral biphosphine catalyst of ruthenium to synthesize chiral indanamine in a cis form with high yield and high stereoselectivity, and then obtaining chiral indanamine in a trans form through a transposition process.The reaction process is as follows: the chiral indanamine in the trans form has a content of greater than 99%, 98% ee and a total yield of greater than 90%, the catalyst is convenient and easy to obtain, the operation is simple, the raw material is easy to obtain, the three-waste pollution is small, the energy consumption is low, and the method is suitable for industrial production.

The invention provides a supported nickel phosphide catalyst as well as a preparation method and application thereof in reductive amination reaction, and relates to the technical field of secondary amine synthesis. The preparation method provided by the invention comprises the following steps: dispersing a composite phosphoric acid carrier in a nickel solution, adding a phosphate solution, carrying out hydrothermal reaction, separating and calcining to obtain a precursor; reducing the precursor in a hydrogen-containing atmosphere to prepare the supported nickel phosphide catalyst; the metal element in the composite phosphoric acid carrier comprises one of cerium and aluminum. According to the method, nickel phosphide can be used for replacing a traditional noble metal catalyst, the catalytic reaction cost is effectively reduced, dependence on noble metal resources is reduced, and conversion of generating bicyclic secondary amine through reductive amination is facilitated.

A method for producing substantially enantiomerically pure (1R,25)-2,6-dimethyl-1-indanamine is described, which comprises reacting a mixture of four stereoisomers of 2,6-dimethyl-1-indanamine with an acylating or carboxylating agent in the presence of a protein having lipase activity, and carrying out the method using dynamic kinetic stereoisomer resolution.