50 results about "Phenylmethylamine" patented technology

The invention provides a novel preparation method of Apalutamide. According to the novel preparation method, 2-fluoro-4-bromo-N-methyl benzene methanamine amide, 1-amino cyclobutyl carboxylate hydrochloride, and the like are taken as initial raw materials, and substitution reaction is carried out so as to obtain 1-((3-fluoro-4-(methyl carbamyl)phenyl)amino) cyclobutane-1-carboxylic acid, wherein synthesis yield is higher than 70%, and purity is higher than 97.2%; then esterification is carried out so as to obtain 1-((3-fluoro-4-(methyl carbamyl)phenyl)amino) cyclobutane-1-carboxylic ester, wherein synthesis yield is higher than 83%, and purity is higher than 97.8%; and at last, ring closing reaction with 2-cyan-3-trifluoromethyl-5-isothiocyano pyridine is carried out so as to obtain Apalutamide, wherein yield is higher than 68%, and purity is higher than 98.1%. The preparation method possesses following advantages: the raw materials are easily available; technology is simple; operationis convenient; yield is high; and cost is low.

The invention relates to chiral beta-arylamine compounds prepared by asymmetric reductive amination reaction and a preparation method of the chiral beta-arylamine compounds. The chiral beta-arylamine compounds are prepared by hydrogenised asymmetric reductive amination reaction under the action of chiral catalysts on the basis of alpha-aryl ketone and aminodiphenylmethane. By the synthesis method, catalyst consumption can be reduced to 5*10<-5>, enantioselectivity of products is up to 98%, and a diaryl methyl group can be removed from N-diaryl methyl-beta-arylamine obtained from the reaction under mild conditions to finally obtain first-grade beta-arylamine, so that the problem of synthesis of the chiral beta-arylamine compounds is solved. In addition, since relevant raw materials are very cheap, the chiral beta-arylamine compounds and the preparation method have extremely high industrial application potential.

The invention relates to a process for producing azelnidipine. A yield improving and refining and purifying method is provided for synthesizing a dihydropyridine calcium antagonist. The process comprises the following steps of: performing N-alkylation cyclization, esterification and Pinner synthesis on epoxy chloropropane and aminodiphenylmethane serving as initial raw materials to obtain 3,3-diaminoacrylic acid-1-diphenylmethyl-3-azetidinyl ester acetate; and performing Hantzsch synthesis with 2-(3-nitrobenzylidene)isopropyl acetoacetate to prepare the azelnidipine, wherein the 2-(3-nitrobenzylidene)isopropyl acetoacetate is obtained by performing Knoevenagel reaction on nitrobenzaldehyde and isopropyl acetoacetate, and alpha-crystal form azelnidipine is prepared by crystal transition. By the process, the defects of a large number of side reactions, high production cost and the like of the foreign process are overcome, the process has the advantages of mild reaction condition, high yield, high product quality, no use of a class 1 solvent benzene, and the like, and the product is further purified.

The invention discloses a PSMA inhibitor, a compound as well as a preparation method and application of the compound. The structure of the compound is shown as a formula A defined in the description, wherein R1 is cyclohexane methylamine or benzylamine, R2 is DOTA(I) or NODA(II) used for complexing (radioactive) metal ions, radioactive metal nuclides are used for diagnosis or treatment, and non-radioactive metal nuclides are used for being combined with radioactive nuclides. The invention also provides a preparation method and application of the compound. The compound has high affinity with prostate specific membrane antigen (PSMA), has the characteristic of rapid removal, and is especially suitable for tumor radionuclide target diagnosis, staging, treatment and the like.

The invention discloses an oxygen reduction catalyst layer based on polyionic liquid as a proton conductor and a preparation method of the oxygen reduction catalyst layer. The method comprises the steps: carrying out copolymerization reaction on styrene monomer and N, N-dimethyl vinyl benzylamine to synthesize a proton-type polyion liquid copolymer; then, taking the copolymer based on the proton-type polyion liquid as a proton conduction layer and an adhesive, performing the ultrasonic dispersion of the copolymer, a catalyst, isopropanol and water, preparing catalyst ink, coating the surface of a glassy carbon electrode with the catalyst ink, and performing natural drying to obtain an oxygen reduction catalyst layer. Compared with the prior art, 1, the cost is lower, and the preparation process is simpler; 2, the catalyst layer has better proton conductivity than the traditional catalyst layer; 3, the novel catalyst layer can obviously inhibit the coverage of non-reactive active oxideson active sites of platinum and effectively enhance the transmission performance of oxygen on a proton conductor nano layer and a platinum interface, so that the oxygen reduction activity of the whole catalyst layer is improved, and the purpose of reducing the platinum loading capacity in the catalyst layer is expected to be achieved.

The invention discloses polyamide thermofuse with a low melting point and a preparation method thereof. A polymerization reaction is conducted by using polyatomic acid and polyamine as reagents, and meanwhile auxiliaries such as modifier, palladium catalyst and defoamer are added; the polyatomic acid is the mixture of oxalic acid, sebacic acid and dodecanedioic acid; the polyamine is the mixture of decamethylene diamine, PA-12 and N-(3-aminopropyl)-N-dodecyl-1; the modifier is the mixture of N-benzyl-4-trifluoromethyl phenylmethylamine and 4,4'-diaminodiphenyl ether; the palladium catalyst isbis(dibenzylideneacetone)palladium or tris(dibenzylideneacetone)dipalladium; and the defoamer is polydimethylsiloxane or ethylene glycol siloxane. The prepared thermofuse has the low melting point, and meanwhile has large intensity and elongation, still has the large intensity and elongation even being irradiated with ultraviolet light for a long time, and can meet actual needs of production and life.

The invention provides a synthetic method of 3-chloro-5-(difluoromethoxy)benzylamine, and belongs to the field of chemical synthesis of medicines. According to the method, 3-chloro-5-hydroxybenzonitrile is used as a raw material, and under the protection of nitrogen, the final product 3-chloro-5-(difluoromethoxy)benzylamine is obtained through difluoromethylation and reduction. The method is reasonable in process design, short in route, simple to operate and easy to control.

The invention provides a method for improving the whiteness of meta-position aramid fiber, and belongs to the technical field of aramid fiber preparation. Benzoyl chloride or benzylamine is added in a low-temperature polycondensation reaction process of m-phenylenediamine and m-phthaloyl chloride for intervention to obtain polycondensation liquid, and then the meta-aramid fiber is prepared through drawing and spinning or fiber precipitation. According to the method, the benzoyl chloride or the benzylamine is added into a mixture of the m-phenylenediamine and the m-phthaloyl chloride for intervention, and during high-temperature treatment in the later processing process of the product, nitrogen protection is performed, so that the prepared meta-aramid fiber is very excellent in high-temperature resistance and flame retardance, and meanwhile, the color is uniform and the whiteness is relatively high; and the whiteness of the aramid fiber prepared through the drawing and spinning method is about 73-78, and the whiteness of the aramid fiber prepared through the fiber precipitation method is about 88-94.

The invention discloses a preparation method of tetraimidazole free alkali. Alpha-[[(2-hydroxyethyl)amino]methyl]benzyl alcohol reacts with thionyl chloride, then water is added for heating dissolution, after activated carbon thermal filtration, N-(2-chloroethyl)-alpha-(chloromethyl)-benzylamine hydrochloride is obtained through cooling crystallization, then N-(2-chloroethyl)-alpha-(chloromethyl)-benzylamine hydrochloride and thiourea are subjected to direct cyclization, and tetraimidazole free alkali is generated. The method is simple in production process, mild in reaction condition and highin total yield, the production cost is reduced, the generation amount of three wastes is small, the double contradiction between economy and environment in the development process of modern enterprises is well solved, and the production process has great competitiveness and good industrial prospects.

The invention discloses an improved antirust cleaning agent. The improved antirust cleaning agent is prepared from the following raw materials in parts by weight: 1.2-3.4 parts of ethylene glycol n-butyl ether, 1.5-3.2 parts of tetramethylenediamine tetramethylene phosphonic acid, 2.3-5.7 parts of turpentine oil, 3.2-5.5 parts of bromo hydrocarbyl dimethyl substituted benzylamine, 6.5-8.7 parts of undecanedioic acid, 6.3-8.4 parts of copper ion blocking agent, 1.2-2.5 parts of surfactant and 3.5-5.5 parts of emulsifier. The metal cleaning agent disclosed by the invention is low in foam and can be used for easily removing difficultly-removed dirt, such as lubricating grease, from metal parts / fittings or mechanical equipment during use; meanwhile, after the metal parts / fittings or mechanical equipment is cleaned, the metal parts / fittings or mechanical equipment can be kept rustless when exposed to the air; the cleaning agent is effective to iron materials, copper materials, aluminum materials and composite metal materials and is relatively low in cost.

The invention relates to a processing technology of a functional nano regenerated fiber. The functional nano regenerated fiber is obtained through wet spinning, and is obtained through the steps of adding a nano function agent into a spinning solution, and then carrying out jet spinning. The nano function agent comprises a rhizoma phragmitis extract, benzylamine, butenedioic acid, ethylphenylamine, ammonium persulphate and deionized water. The main component of the rhizoma phragmitis extract is phenolic acids; and under the action of the ammonium persulphate as a catalyst, the rhizoma phragmitis extract, the benzylamine and the butenedioic acid form an early shrinkage body. The ultraviolet resistance, the antimicrobial property and the breaking strength of the regenerated fiber are improved; and the breaking strength can reach up to be more than 300N.

The invention provides a preparation method of tetraimidazole hydrochloride, which comprises the following steps: preparing tetraimidazole; the preparation method comprises the following step: reacting tetraimidazole, 1, 2-dibromoethyl benzene and 2-aminothiazoline hydrochloride to generate tetraimidazole. The synthetic route is shorter, the comprehensive yield is higher than that of other processroutes, styrene is used as an initiator, tetra-imidazole free alkali is used as a final product, the yield of the hydroxysalt process route is about 65%, the yield of the N (2chloroethyl) alpha (chloromethyl) benzylamine hydrochloride process route is about 72%, and the yield can reach 85% or above when the patent route is used. Meanwhile, the problem of large amount of waste water and waste saltgenerated by multi-step reactions such as chlorination, hydrolysis and cyclization is avoided, the investment of reaction equipment such as an autoclave is avoided, the green chemical engineering requirement is met, the economic benefit is remarkable, and the industrial prospect is good.

The present invention relates to a new method of making phenalkamines, products produced by such method, and use of such products. The method provides for phenalkamines obtained by an amine exchange reaction of a cardanol derived Mannich base with a compound with at least one alkylene or aralkylene group and at least two amino groups. These products may be used to cure, harden, and / or crosslink an epoxy resin. The curing agent compositions of this invention are of low viscosity and can be used neat or dissolved in a minimum amount of an organic solvent or diluent to effect cure of epoxy resins.

A solid adhesive is described that has an excellent finish, a light coating feeling, and is also capable of adhering to paper, wood, cloth, and the like. The solid adhesive contains water, an organic solvent, a gelation agent such as a dibenzalide of pentavalent to hexavalent sugar alcohol, and a polyvinyl formal resin. In some examples, the solid adhesive further includes a polyvinyl butyral resin and / or an adhesive resin such as a polyvinyl pyrrolidone resin. A feed type solid adhesive may be provided, including a feeding container that is filled with the solid adhesive described above.

The invention discloses a method for dynamic kinetic resolution of alpha-aryl-alpha-alkyl carboxylic ester and application, and belongs to the technical field of organic synthesis. Pentafluorophenol ester and benzhydrol are taken as reactants, a dynamic kinetic resolution reaction is carried out under the nitrogen-oxygen catalysis of chiral DMAP derived from diphenylmethylamine to obtain alpha-aryl-alpha-alkyl ester, and (S)-naproxen, (S)-ibuprofen, (S)-ketoprofen, (S)-fenopolfen and (S)-flurbiprofen are synthesized. According to the chiral DMAP nitrogen-oxygen catalyst, oxygen atoms in pyridine nitrogen-oxygen serve as nucleophilic sites to participate in a dynamic kinetic resolution reaction, and meanwhile hydrogen in catalyst molecules also plays a key role. The method has the advantages of good yield, high enantioselectivity and the like.

The invention belongs to the technical field of photocatalytic oxidation, and particularly relates to a method for preparing N-benzylidenebutylamine through efficient photocatalytic oxidation of benzylamine. A flavin photosensitizer is used as a catalyst, and N-benzylidenebutylamine is prepared by a one-step method under the action of illumination. The preparation method specifically comprises the following steps: (1) dissolving the flavin photosensitizer and benzylamine in an organic solvent; and (2) introducing air into the mixed solution obtained in the step (1) at room temperature and normal pressure, and performing illumination to obtain the N-benzylidenebutylamine. The preparation process is simple, the preparation conditions are mild, no heavy metal is used in the preparation process, the preparation method is environment-friendly, and the cost is low; according to the method provided by the invention, N-benzylidenebutylamine can be prepared under the conditions of normal temperature and normal pressure, the energy consumption is low, the method is simple and easy to operate, and the method can be used for large-scale production.

The invention relates to a synthesis method of 8-amino-1-{[2-(trimethylsilyl) ethyoxyl] methoxy} octane-3-ketone, and belongs to the technical field of chemical synthesis of medicines. The method comprises the following steps: protecting diphenylmethylamine by N-Boc, reacting with sodium hydride to obtain a sodium salt intermediate, and carrying out substitution reaction on the sodium salt intermediate and 1, 5-dibromopentane to obtain an intermediate-1; preparing a zinc bromide intermediate from the intermediate-1, enabling the zinc bromide intermediate to react with 3-{[2-(trimethylsilyl) ethyoxyl] methoxy} methyl propionate to generate an intermediate-2, and carrying out catalytic hydrogenation deprotection reaction on the intermediate-2 to obtain the lipoic acid intermediate, namely 8-amino-1-{[2-(trimethylsilyl) ethyoxyl] methoxy} octane-3-ketone. The method has the advantages of mild process conditions, easily available raw materials and high purity of each intermediate, is beneficial to quality control and improvement of raw material medicine production, and is suitable for industrial production.

The invention relates to a preparation method of N-phenylmethyl benzylamine, which is characterized by comprising the following steps of by using polyoxometallate as a catalyst, putting into a reaction container, sequentially adding an organic solvent, benzylamine and benzoic acid into the container, finally adding an additive, heating, stirring, reacting, and separating to obtain the N-phenylmethyl benzylamine. After the reaction is finished, the catalyst can be recycled, the system after the reaction is finished is directly filtered, the polyoxometallate can be directly filtered out and recycled after being treated, and the recycled polyacid is used for preparing the N-phenylmethyl benzylamine. Compared with the prior art, the method has the advantages that benzylammonium and benzoic acid can react to prepare N-phenylmethyl benzylamine, high activity and high selectivity are achieved, reaction conditions are mild, environment friendliness is achieved, the catalyst can be recycled, and great industrial production potential is achieved.

The invention discloses rapidly cross-linked and cured MQ type silicon resin as well as a preparation method and application thereof. In order to overcome the defects that the existing MQ type silicon resin cannot be cross-linked and cured or a noble metal platinum complex needs to be used during cross-linking and curing or organic tin and organic titanate compounds which have great influence on the environment are used as catalysts, the curing temperature is high and the curing time is long, the invention provides a preparation method of the MQ type silicon resin. According to the invention, the alpha-cyano propyl acyloxyethyl oxypropyl terminated MQ silicon resin is designed and can be quickly crosslinked and cured at room temperature and in the air, and when a small amount of N, N-dimethyl p-benzylamine is added as an accelerant, the alpha-cyano propyl acyloxyethyl oxypropyl terminated MQ silicon resin can be quickly crosslinked and cured within 10s. The organosilicon material formed after cross-linking and curing has no obvious crystallization peak, melting peak and glass transition temperature in the range of-120 to 120 DEG C, has good structural stability, and has good application prospects in the fields of rapid shaping, rapid bonding and the like.

The invention discloses a method for transferring C=N double bonds by chlorella, which belongs to the field of chemistry, and can solve the problems of certain pollution to the environment and highercost due to the use of acid or alkali in the existing double bond transfer method, and diphenyl methylamine is very active primary amine and is easy to react with aldehyde and ketone to generate Schiff base, so that the diphenyl methylamine can be used as an active aminating agent for preparing other amines. According to the method, diphenyl methylamine and furfural are used for forming Schiff base, then chlorella is added, and [1, 3]-proton transfer can be promoted through illumination. The method is environment-friendly and low in cost, the chlorella is easy to culture and obtain, and acid or alkali which easily causes pollution is not used.

The invention provides a method for preparing a benzylamine compound through photocatalysis. The method comprises the step of enabling an aromatic aldehyde compound to react with ammonia water through a photocatalyst under the conditions of illumination and inert gas to obtain the benzylamine compound. The method for preparing the toluidine compound through photocatalysis can be used for replacing an existing mature organic synthesis process, conditions are mild, selectivity is high, universality is achieved, and the method is suitable for industrial production.

The invention provides a preparation method of polaprezinc and a polaprezinc preparation. The preparation method of polaprezinc comprises the steps that benzylamine, 3-halopyruvic aldehyde, a first acid reagent and a first organic solvent are mixed for a reaction, then ammonium halide and polyformaldehyde are added, and 1-phenylmethyl-4-(halomethyl)-1H-imidazole is obtained through a reaction; thematerial is added in a reaction mixture of 2-aminoacetonitrile, an alkaline reagent and a second organic solvent, and the materials are reacted to obtain 3-amino-nitrogen-(2-(1-phenylmethyl-1H-4-imidazole)-1-cyanoethyl) propanamide; the material is mixed with a reducing agent, a second acidic reagent and a third organic solvent, and the materials are reacted to obtain 3-amino-nitrogen-(1-carboxyl-2-(1hydrogen-4-imidazole) ethyl) propionamide; and the obtained product and zinc salt are dissolved in a fourth organic solvent, and a reaction is carried out to obtain the polaprezinc. According tothe technical scheme, almost no pollution is caused to the environment, no potential safety hazard exists in the preparation process, the steps are short, the conditions are simple, purification is easy, the yield is high, the preparation cost of the polaprezinc is low, and the polaprezinc is suitable for industrial production.

A beneficiation agent for copper-lead flotation of copper-lead ore and a preparation method thereof, which is made of the following raw materials in parts by weight: 10-20 oleic acid, 5-8 sodium carbonate, 30-50 sodium sulfide, 10-15 sulfur, ester Xanthophyll 12‑18, carbon disulfide 20‑40, quicklime 1‑2, p-benzylamine 30‑60, activator 4‑5, phenylethyl alcohol 20‑35. The present invention has the characteristics of high sorting efficiency, high yield, less dosage, simple and reliable technological process, easy operation, etc., is suitable for the application of copper-lead flotation in copper-lead ore, and can bring good economic benefits to the copper-lead ore. benefit.

The invention provides a preparation method of azelnidipine starting material ethylamine benzhydrylamine. The method comprises the step of using benzophenone and formamide as raw materials to carry out aLeuckart reaction. The catalyst of silicon dioxide is added into a reaction system, and thus the reaction time is drastically reduced, wherein the time is decreased to 3-4 h from 8 h, and therefore energy consumption is significantly reduced; the rough product yield of a compound II is dramatically increased and is up to 96-98%. The purity of HPLC is not lower than 96.5%, so that it is ensured that after the ethylamine benzhydrylamine obtained by hydrochloric acid hydrolysis is purified once, the yield can reach 80%, the purity is not lower than 99.9%, and the ethylamine benzhydrylamine is quite suitable for industrial production.

The invention belongs to the field of synthesis of pesticide intermediates, and provides a method for catalytically synthesizing 4-(4-methylphenoxy) benzylamine by utilizing modified nano nickel. The preparation method specifically comprises the following steps: (1) stirring and mixing a solvent, a metal nickel salt, a polyhydric alcohol type nonionic surfactant, a reducing agent and an alkali solution, and performing ultrasonic treatment to prepare modified nano nickel; (2) adding water, potassium hydroxide, p-cresol, an organic solvent and p-chlorobenzonitrile into a reaction kettle, and stirring for reaction to prepare 4-(4-methylphenoxy) benzonitrile; and (3) adding ammonia water, ethanol, the modified nano nickel and 4-(4-methylphenoxy) benzonitrile into a high-pressure kettle, and introducing hydrogen to prepare the 4-(4-methylphenoxy) benzylamine. Compared with the prior art, the modified nano nickel catalyst used in the invention has the advantages of small particle size, high catalytic efficiency, good reusability and the like, and the production efficiency of the product is improved.

The invention provides a preparation method of levocetirizine. The method comprises the following steps of: the step 1, carrying out a cyclization reaction on (R)-4-chlorodiphenyl methylamine and tris(2-chloroethyl)amine to obtain a compound represented by a formula (I); 2, performing condensation reaction of the compound shown in the formula (I) and 2-ethyl glycolate to obtain a compound shown ina formula (II); and the step 3, converting the compound shown in the formula (II) into levocetirizine. According to the preparation method, (R)-4-chlorodiphenyl methylamine and tris(2-chloroethyl)amine are taken as the initial raw materials, and cyclization reaction, condensation reaction and hydrolysis reaction are carried out so as to obtain levocetirizine. The synthetic route provided by the invention is short, the yield is high, and experimental results show that the yield of the levocetirizine prepared by the method provided by the invention can reach 47%, and the purity can reach 99.7%.

The invention relates to a method for recovering 3-ethoxy-4-methoxy-α-[(methylsulfonyl)methyl]-benzylamine, which belongs to the technical field of chemical synthesis. The technical scheme of the present invention is as follows: first, compound I, a by-product of the product, is free to recover compound III, and intermediate II is subjected to deamination reaction to generate intermediate IV, and then intermediate IV is subjected to an addition reaction to generate compound V. The beneficial effects of the present invention are: (1) the synthetic method of the present invention successfully recycles the by-products after splitting, preventing the generation of solid waste and reducing environmental pollution; (2) the synthetic method of the present invention The by-products after dismantling were successfully recycled and reused, which reduced the production cost from the original 1504 yuan / kg to 1002.67 yuan / kg. After continuous production, the cost will continue to be reduced.

A method for synthesizing 8-amino-1-{[2-(trimethylsilyl)ethoxy]methoxy}octane-3-one belongs to the technical field of pharmaceutical chemical synthesis. Steps: first protect benzhydrylamine with N-Boc, and then react with sodium hydride to obtain its sodium salt intermediate, which is subjected to a substitution reaction with 1,5-dibromopentane to obtain intermediate-1; intermediate ‑1 yields the zinc bromide intermediate, which is subsequently reacted with methyl 3‑{[2‑(trimethylsilyl)ethoxy]methoxy}propionate to yield intermediate ‑2, which is decomposed by catalytic hydrogenation Protection reaction, obtain lipoic acid intermediate 8-amino-1-{[2-(trimethylsilyl)ethoxy]methoxy}octane-3-one. The technical process conditions are mild, the raw materials are easy to obtain, and the purity of each intermediate is high, which is beneficial to the quality control and improvement of the production of raw materials, and is suitable for industrial production.

The invention provides a synthesis method of a rivastigmine optical isomerization intermediate and (R)-rivastigmine. The method comprises the following steps: carrying out an asymmetric reductive amination reaction on 3-nitromethyl ethyl formate acetophenone and diphenyl methylamine under the catalysis of an Ir complex to obtain the rivastigmine optical isomerization intermediate, carrying out a metal debenzylation catalysis reaction on the rivastigmine optical isomerization intermediate in a hydrogen atmosphere to obtain a compound 3, and carrying out an Eschweiler-Clarke methylation reactionon the compound 3 and formaldehyde to obtain the (R)-rivastigmine. The synthesis method of the (R)-rivastigmine has the advantages of short synthetic steps, high yield, high efficiency, economical property, practicability, environmental friendliness and good atom economy.

A beneficiation agent for tantalum-niobium ore flotation tantalum-niobium, made of the following raw materials in parts by weight: diesel oil 10-15, sodium carbonate 15-40, sodium acetate 20-30, ammonium chloride 15-25, 2-methyl Butyric acid 12‑18, quicklime 1‑2, p-benzylamine 30‑60, activator 4‑5, phenylethyl alcohol 20‑35. The invention has the characteristics of high sorting efficiency, high yield, less consumption, simple and reliable technological process, easy operation and the like, and is suitable for the application of tantalum-niobium ore flotation.