85results about "Preparation by reductive alkylation" patented technology

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.

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.

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 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 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.

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 discloses a heterogeneous cobalt-based coordination catalyst as well as a preparation method and application thereof. The cobalt-based catalyst comprises a carrier and an active component, the active component is a cobalt species, and the carrier is an oxide / molecular sieve / carbon material. The heterogeneous cobalt-based coordination catalyst is obtained by coordinating an ionic liquid and a metal salt, loading the coordinated ionic liquid and metal salt on a carrier and calcining the carrier. The cobalt species in the catalyst exist in the form of cobalt nanoparticles and cobalt-Nx, and can promote the aldehyde reductive amination reaction to generate primary amine with high selectivity. The catalyst adopted by the invention is environment-friendly, small in dosage and excellent in catalytic performance, can realize high-selectivity and high-yield synthesis of primary amine by catalyzing the aldehyde reductive amination reaction, and has the advantages of mild reaction conditions, easiness in separation and recovery and the like.

The invention discloses a method for photocatalytic synthesis of polydeuterium substituted amine, and relates to the technical field of chemical synthesis. The method comprises the step of reacting a carbonyl compound with an amine compound in the presence of a deuterium-containing reagent, a mercaptan catalyst and a reducing agent under the conditions of a photocatalyst and illumination to obtain the polydeuterium substituted amine. According to the method disclosed by the invention, multiple introduction of deuterium atoms at alpha-carbon sites of a target amine product is realized through a series free radical mechanism initiated by photon-generated carriers, so that simple and easily available raw materials are directly converted into the polydeuterium substituted amine. According to the invention, the ubiquitous problems that only one deuterium atom can be introduced to a nitrogen alpha-site, the synthesis route is tedious, the operation steps are complicated and the existing deuterated amine synthesis technology depends on an expensive deuterium source or a metal catalyst are solved; the invention provides a novel polydeuterium substituted amine synthesis strategy which has the advantages of simple steps, mild conditions, high atom economy and easiness in large-scale production.

The invention relates to a new method for producing twin-tail triamines, preferably fatty twin-tail triamines. Furthermore, the present invention relates to the production of diamines obtained from internal ketones. These diamines may be used in the method for producing twin-tail triamines according to the invention. Finally, the invention relates to a new aldehyde compound, which is an intermediate product of the method for producing twin-tail triamines of the invention.

The invention discloses a triaminobenzene derivative as well as a preparation method and application thereof, and the compound is obtained by reacting 1, 3, 5-triaminobenzene with ketone in the presence of hydrogen. Through molecular structure design, conditions or carriers for generating a benzoquinone structure are essentially eliminated. The triaminobenzene derivative disclosed by the invention is a novel green anti-aging agent, has lower migration performance and extraction resistance, and can prolong the service life of a rubber product and avoid environmental pollution; the migration rate in rubber is lower than that of a traditional anti-aging agent, so that the later-stage anti-aging performance of the anti-aging agent can be better ensured.

The present application relates to a kind of catalyst and its preparation method and application, belong to catalytic field.The catalyst includes metal-based active component and surface metal oxide active component;The metal-based active component includes at least one of nickel-based catalyst or cobalt-based catalyst;The surface metal oxide active component includes at least one of tungsten oxide or molybdenum oxide deposited on the surface of metal-based active component.The catalyst can be used for the preparation of multistage amine, and its operation is simple.The catalyst has high activity, high safety, high selectivity and good stability for reduction amination reaction, can be repeatedly used, is conducive to improving the quality and quality stability of product, reduces process cost, modification cost is low, is conducive to large-scale production.

The present application relates to a kind of nickel catalyst, preparation method.The nickel catalyst includes the structure formed by the chemical bond effect of metal-based active center and formate ligand, the metal-based active center is nickel, formate is combined with nickel with bidentate coordination structure;The nickel catalyst of the present application has higher cyclohexylamine yield, when realizing the conversion rate of 100% of cyclohexanone, the yield of product cyclohexylamine can be up to 96.45% at most;Preparation method is simple, catalyst preparation process is simple, easy to operate, and various aids do not need to be added in catalytic process, reduce the complexity of reaction system, it is favorable to the purification of product, suitable for industrial application.

A method for making a di(aminoaryl)fluorene compound that includes the steps of: (a) reacting a fluorenone compound according structure (I):with excess aminobenzene according to structure (II):wherein: each R1, R2, R3, R4, R12, and R13 is independently a group that is inert in the polymerization of epoxy compounds, and R11 is H or (C1-C6)alkyl, in the presence of an acid catalyst, in a liquid medium comprising an aromatic or substituted aromatic solvent having a boiling point of greater than or equal to 150° C. and from which the di(aminoaryl)fluorene compound is crystallizable, to form a crude product mixture comprising the di(aminoaryl)fluorene compound, (b) crystallizing di(aminoaryl)fluorene compound in the product mixture, and (c) separating the product mixture into crystallized di(aminoaryl)fluorene compound and a filtrate.

The invention relates to the technical field of catalysts, in particular to a pretreatment method and application of a ketoamine reductive alkylation reaction catalyst. The dilute atmosphere containing nitrous oxide is adopted to perform pressurization treatment on the catalyst, and vacuum degassing and hydrogen reduction treatment are matched, so that the generation of by-products higher than the boiling point of the product can be effectively inhibited while the original activity and selectivity of the catalyst are not sacrificed, and the product purity is improved. The catalyst treatment method provided by the invention is carried out in situ in a reactor without unloading and transferring, the operation method is simple, the treatment cost is low, and a p-phenylenediamine antioxidant product prepared from the treated catalyst has the characteristics of light color, high purity and excellent quality.

The present invention relates to a process for the preparation of enantiomerically and diastereomerically enriched cyclobutane amines and amides by reacting (a) cyclopropylcarbonitrile to a cyclopropylcarbaldehyde, (b) further reacting to a cyclobutanone, or (d') further reacting to an enamide, 5 (c) further reacting to enantiomerically and diastereomerically enriched cyclobutane amines, or (d) further reacting to an enamide and (e) to an enantiomerically and diastereomerically enriched cyclobutylamide to obtain (f) an enantiomerically and diastereomerically enriched cyclobutane amine, and (g) further reacting to an enantiomerically and diastereomerically enriched cyclobutane amide.

The application relates to a preparation method of bromhexine hydrochloride, which comprises the following steps: adding 3,5-dibromo-o-amino benzaldehyde, N-methyl cyclohexylamine and a water absorbent into a reaction solvent, stirring under a protective atmosphere, adding a reducing agent in batches at low temperature, continuing to stir under the condition of rising to room temperature, adding a quenching solvent after the reaction is completed, performing suction filtration, rotating and drying the filtrate, adding purified water and an organic solvent, adding concentrated hydrochloric acid under the condition of room temperature to adjust the pH to 0.5-4.0, stirring, performing suction filtration, washing, drying and obtaining bromhexine hydrochloride. The preparation method provided by the application is high in yield and purity, mild in conditions, simple in operation and suitable for industrialized production.

Belonging to the technical field of organic synthesis, the invention relates to an efficient synthesis method of trifluoromethoxycarb, which comprises the following synthesis steps: taking a 3-methyl-2-butanone compound as a raw material for bromination to obtain 1-bromo-3-methylbutane-2-ketone; the method comprises the following steps: carrying out reductive amination on 1-bromine-3-methyl butane-2-ketone under the catalysis of transaminase to obtain (s)-1-bromine-3-methyl butane-2-amine; the (S)-1-bromine-3-methyl butane-2-amine is subjected to condensation with trifluoroethyl chloroformate, and 2, 2, 2-trifluoroethyl (s)-(1-bromine-3-methyl butane-2-yl) carbamate is obtained through condensation of the (S)-1-bromine-3-methyl butane-2-amine and trifluoroethyl chloroformate; the preparation method comprises the following steps: carrying out substitution reaction on 2, 2, 2, 2-trifluoroethyl (s)-(1-bromo-3-methylbutane-2-yl) carbamate and 4-methyl benzyl to obtain the trifluoromethoxycarb. The synthesis process is simple, efficient, green and safe.

This invention discloses a method for preparing amine compounds from biomass-derived aldehydes via photocatalysis, belonging to the field of photocatalytic organic synthesis technology. This method requires no additional hydrogen-donating reagent for amine compound preparation. Under light irradiation, through the synergistic effect of a photocatalyst and a metal co-catalyst, amine compounds are synthesized from ammonia via the reaction of biomass-derived aldehydes without the need for additional organic hydrogen-donating reagents. This method can be carried out at room temperature and pressure, has high yield, is environmentally friendly, and is suitable for industrial production.