35 results about "Amine synthesis" patented technology

The application relates to the field of catalytic synthesis, and discloses a methylamine synthesis method, which comprises the following steps: reacting methanol and ammonia in the presence of a zeolite catalyst treated by an organic alkali to generate a methylamine-containing stream; the acid amount of the zeolite catalyst treated by the organic alkali is 200-400 mu mol.g ‑1 The methylamine synthesis method can reduce the selectivity of trimethylamine in the reaction product, reduce the content of trimethylamine in the product, and ensure high methanol conversion rate.

The invention belongs to the technical field of disease and pest control, discloses application of tyrosine hydroxylase as a target spot in prodenia litura pest control for the first time, screens out a dopamine synthesis inhibitor AMPT aiming at tyrosine hydroxylase, and develops a technology for efficiently controlling prodenia litura. According to the technology, AMPT is injected into the fourth-instar larvae of the prodenia litura, and the melanin deposition of the exoskeleton of the larvae is reduced, the color of the body surface becomes light and the athletic ability is remarkably reduced by utilizing the dopamine synthesis inhibition function of AMPT. On one hand, reduction of melanin deposition weakens the environmental adaptability of pests, and the exposure risk of the pests in the natural environment is increased; on the other hand, the migration behavior of the pests is directly influenced by the decline of the exercise ability, and the population diffusion and hazard range of the pests are limited. The dual-action mechanism reduces the environmental adaptability and survival competitiveness of the pests, and provides a new strategy for green prevention and control.

The present application relates to the technical field of compound synthesis, and in particular to a preparation method of amino acid-based lactam, comprising: A) reacting an alpha-amino acid and an alpha-hydroxy acid ester in a first solvent under the action of a first catalyst to obtain N-(hydroxyacyl)-amino acid ester; B) reacting the N-(hydroxyacyl)-amino acid ester in a second solvent under the action of a second catalyst to obtain amino acid-based lactam with a structure shown in Formula I; in Formula I, R1 and R2 are independently selected from one of hydrogen, a C1-C4 straight-chain or branched-chain aliphatic hydrocarbon group, a substituted or unsubstituted C6-C30 aryl group, a protected amino group, a protected carboxyl group, a protected hydroxyl group and a protected sulfydryl group; and the protecting group is one of an alkoxycarbonyl group, an acyl group and an alkyl group. The present application can solve the problems in the existing lactam synthesis process, such as high raw material risk, complicated process, and difficult product purification.

A method for the catalytic reduction of amides to amines belongs to the field of amine synthesis. The method involves the direct catalytic reduction of tertiary and secondary amides to amines using reagents such as iridium and silanes. The steps are as follows: In an organic solvent, the amide and silane are reacted under the catalysis of an iridium complex and an acid, followed by concentration and purification to obtain the amine. The molar ratio of amide:iridium complex:acid:silane is 1:0.0000001–0.001:0.1–1:2–4. This invention uses stable and readily available amides as raw materials and achieves high-efficiency synthesis of amines with very low catalyst loading, using an iridium complex and a low-valence acid. The steps of this invention are simple to operate and separate, the reaction rate is fast, the reaction conditions are mild, and the reagents used are all inexpensive and readily available commercial reagents. The yield is high, and the functional group tolerance is good.

Provided are a transaminase and a variant thereof, and the use of the transaminase and the variant thereof in amine synthesis.

The application discloses a linear drainage ditch for rural areas and a permeation testing method thereof, relates to the technical field of sewage collection, and solves the problems of high use cost and easy damage of the existing concrete drainage ditch for rural areas, reduces the material consumption, and reduces the construction difficulty, and the specific scheme is as follows: the drainage ditch main body is provided with a grid on the groove, the drainage ditch main body is made of a mixed material, the main agent of the mixed material is epoxy resin, the curing agent is modified amine T31 synthesized by phenol, formaldehyde and fatty amine, the diluent is acetone, the toughening agent is dibutyl phthalate, the filler is fly ash, and the aggregate is fine aggregate produced by using construction waste.

This application relates to the field of catalyst technology, and more specifically, to a method for preparing a composite catalyst for the synthesis of piperoethylamine, an intermediate of berberine. The method for preparing the composite catalyst for the synthesis of piperoethylamine, an intermediate of berberine, includes the following steps: 1) mixing a nickel source and a cerium source uniformly in water, then adding aminotrimethylenephosphonic acid and mixing uniformly to obtain a mixed solution; 2) mixing the mixed solution obtained in step 1), a PVA solution, and SBA-15 powder uniformly, impregnating, and freeze-drying to obtain a lyophilized powder; 3) heating the lyophilized powder obtained in step 2) to 400-500℃ in a nitrogen atmosphere, calcining for 3-5 hours, cooling to 30-60℃; then heating to 530-700℃ in a reducing atmosphere and holding for 2-3 hours, followed by cooling to obtain the final product. The composite catalyst prepared in this application can significantly improve the conversion rate of piperoacetonitrile and the selectivity of piperoethylamine.

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 discloses a synthesis method of an N, N-alkyl substituted amine compound, which utilizes an optimized Gabriel amine synthesis method, and directly uses phthalimide in the presence of alkali, thereby saving the step of converting the phthalimide into sylvite.

The application discloses a method for separating bismuth from actinium, which comprises the following steps: passing a hydrochloric acid or nitric acid solution containing actinium through a cation exchange column, and eluting the cation exchange column with first hydrochloric acid to obtain an eluate containing bismuth (Bi); passing the eluate containing Bi through a TK201 resin column to obtain Bi adsorbed on the TK201 resin column; and eluting the Bi adsorbed on the TK201 resin column with second hydrochloric acid or nitric acid to obtain a Bi eluate. The application uses TK201 resin as a purifying material of Bi for the first time, the TK201 resin is synthesized based on a tertiary amine and doped with a small amount of long-chain alcohol, has specific adsorption on Bi under the condition of a certain concentration of hydrochloric acid, and has no adsorption capacity on Ac and Fr, so that the content of Ac in Bi is greatly reduced.

The present application relates to a kind of 2-isopropyl-4-methylpyridine-3-amine synthesis process, with nickel catalyst, Grignard reagent, to carry out one-step Kumada coupling reaction to obtain product 2-isopropyl-4-methylpyridine-3-amine with 2-chloro-3-amino-4-methylpyridine as starting material.The synthesis process of 2-isopropyl-4-methylpyridine-3-amine of the present application, step is short, raw material is easy to obtain, and does not need to use expensive palladium metal catalyst, cost is low, yield is high, process is simple, three wastes are less, suitable for industrial amplification production.

The invention discloses a synthesis process and a synthesis device of clothianidin, and relates to the technical field of clothianidin synthesis, the synthesis device comprises a four-in-one reactor and a preheating cylinder, the four-in-one reactor comprises a stirring mechanism, a vacuum mechanism, a nitrogen valve, a charging valve and a jacket and filtering mechanism, the nitrogen valve is installed on the outer side of the four-in-one reactor, and the charging valve is installed on the outer side of the four-in-one reactor; one end of the jacket is fixedly connected with a third pipeline, the other end of the jacket is provided with a first pipeline, the outer side of the preheating cylinder is fixedly sleeved with a preheating sleeve, and the interior of the preheating cylinder is rotationally connected with a rotating column through a bearing. According to the present invention, the 1, 5-dimethyl-2-nitroiminohexahydro-1, 3, 5-triazine is adopted to replace the 1, 5-dimethyl-2-nitroiminohexahydro-1, 3, 5-triazine to prepare the clothianidin, such that the reaction yield can be improved by more than 10%, and the yield is stable; side reactions are reduced, and the product has few impurities and high purity.

The application provides a coordination metal catalyst, a preparation method and application thereof, a hindered amine and a preparation method thereof. The preparation method of the coordination metal catalyst comprises uniformly mixing a first metal salt and a second metal salt, then adding an amide-substituted benzene, standing, drying to obtain the coordination metal catalyst; the metal element in the first metal salt comprises one of Co, Pd and Ni or a combination of two or more thereof; the second metal salt is triflate and / or chloride. The application further provides the coordination metal catalyst obtained by the above preparation method and a hindered amine catalyst comprising the coordination metal catalyst. The application further provides the hindered amine and a preparation method thereof, which is prepared by using the above hindered amine catalyst. The coordination metal catalyst provided by the application has the advantages of low cost, high catalytic activity, mild reaction conditions and the like, and can be used for the hindered amine and other reactions related to alcohol amine synthesis.

The application discloses a synthesis method of a conjugated diene amide with a full (E) configuration, and belongs to the technical field of conjugated diene amide synthesis. The application realizes the conversion of an unsaturated aldehyde into a conjugated diene carboxylic acid ester by keeping the double bond configuration of the (E)-unsaturated aldehyde as a raw material, the double bond migration of a phosphoryl intermediate is used, the configuration isomerization in the traditional method is avoided, the product configuration is single, continuous reaction reduces separation loss, the total yield is about 20% higher than that of the prior art, the reaction condition is mild, and the method is suitable for industrial production.

The application belongs to the technical field of synthesis of medical intermediates, and particularly relates to a synthesis method of a chiral intermediate of atorvastatin calcium. 1,3-propanediol is used as raw material, a silicon-based protection reaction is carried out, and then oxidation is carried out, a ring addition reaction occurs under the catalysis of a chiral catalyst and a lithium salt, and a first chiral center is introduced; then, t-butyl acetate is added to carry out a ring opening reaction, a Narasaka-Prasad reduction reaction is carried out to induce a second chiral center; 2,2-dimethoxypropane is added to protect cis diol, finally, tetrabutylammonium fluoride is added to remove the silicon-based reaction, and a Fukuyama amine synthesis method is used to replace the hydroxyl group with the amino group to obtain the chiral intermediate of atorvastatin calcium. The application uses 1,3-propanediol which is cheap and easy to obtain as raw material, and various dangerous, toxic and expensive drugs are not used in the synthesis route process, the method has a simple route, high yield and good repeatability, and can be used for industrial production.

The application provides a method for synthesizing oxazolidinone compounds based on carbon dioxide and alcohol amine, a catalyst, oxazolidinone compounds prepared based on carbon dioxide and alcohol amine, and application of cerium-based composite oxides in preparation of oxazolidinone compounds based on carbon dioxide and alcohol amine. The method comprises the following steps: taking carbon dioxide and alcohol amine as raw materials, and allowing the alcohol amine to react with the carbon dioxide under the action of a solid catalyst to generate the oxazolidinone compounds; wherein the solid catalyst comprises cerium-based composite oxides, and the reaction process comprises liquid-phase carboxylation and cyclization dehydration. The method provided by the application can easily separate the catalyst from the product, and can make the alcohol amine have a high conversion rate.

The invention relates to the field of catalytic synthesis, and discloses a methylamine synthesis catalytic material grading system and a methylamine synthesis method.The grading system comprises a first catalytic material and a second catalytic material which are sequentially arranged in the material flow direction; wherein the volume ratio of the first catalytic material to the second catalytic material is 0.1-3; the first catalytic material is selected from at least one of aluminum oxide, titanium dioxide and bentonite; the second catalytic material comprises zeolite, optionally alumina, and optionally silica. By adopting the grading system, the tolerance of the catalyst can be improved, the long service life of the catalyst is guaranteed, methanol reaction is catalyzed to generate a methylamine product, and the high methanol amination utilization rate is achieved.

The invention relates to the technical field of organic synthetic chemistry, and particularly discloses a synthesis method of o-chlorobenzylamine. According to the method, o-chlorobenzyl chloride, liquid ammonia and caustic soda liquid are used as raw materials, and the preparation process mainly comprises the steps of amination reaction, liquid ammonia recovery, alkali treatment deamination and product purification. Specifically, in a high-pressure reaction kettle, liquid ammonia is used as a reaction medium and reacts with o-chlorobenzyl chloride under the conditions of low temperature and specific pressure, and after the reaction, the liquid ammonia is evaporated out and recycled for recycling; dissolving with water, adding alkali for dissociation, and removing residual ammonia gas under negative pressure; and finally, separating an organic phase by standing and layering, and dehydrating and filtering to obtain a high-purity o-chlorobenzylamine product. According to the method, by constructing a solvent-free system and cooperatively controlling the reaction temperature, the material proportion and post-treatment parameters, side reactions are remarkably inhibited, and therefore high-selectivity synthesis is achieved. The whole process has the advantages of simplicity and convenience in operation, environmental friendliness, high resource utilization rate and easiness in industrial implementation.

The application belongs to the technical field of medicine preparation, and particularly relates to a synthesis method of beta-trifluoromethylthio amide participated by silver trifluoromethylthiol, and the specific steps are as follows: in step 1, acrylamide, silver trifluoromethane thiol, acid and solvent are put into a thick-walled pressure-resistant tube for reaction, the reaction time is 8h, and the reaction temperature is 40-60 DEG C; in step 2, after the reaction is completed, dichloromethane is added to dilute the reaction solution, the organic solvent is removed by rotary evaporation, and the remaining product is separated by column chromatography to obtain beta-trifluoromethylthio saturated amide. By using the method in the application, the preparation of beta-trifluoromethylthio saturated amide can be realized in one step, the operation process is simple, the reaction efficiency is effectively improved, in addition, the reaction temperature is only 40-60 DEG C, and the method has the advantages of low reaction energy consumption, low overall production cost and high degree of technical environmental friendliness.

The invention relates to the technical field of ZSM-5 molecular sieves, in particular to an amine-free synthesis method of a high-silicon ZSM-5 molecular sieve, which is characterized by comprising the following steps: mixing tetraethoxysilane and concentrated hydrochloric acid, hydrolyzing to form silica sol, adding tetrapropylammonium hydroxide, and carrying out hydrothermal crystallization to obtain nanocrystal seed colloid; dissolving aluminum sulfate in water, then adding mixed alkali, then slowly adding water glass, and then adding tetraethoxysilane and the nanocrystalline seed colloid for aging treatment to prepare synthetic gel; performing staged dynamic crystallization treatment on the gel; and carrying out ion exchange to obtain the hydrogen type ZSM-5. According to the amine-free synthesis method of the high-silicon ZSM-5 molecular sieve, a nucleation site is provided by a nano seed crystal, and a template agent is replaced by seed crystal induction; sodium silicate and tetraethoxysilane are adopted as a mixed silicon source, the water-silicon ratio of a system is reduced, the solid content of slurry is increased, meanwhile, mesoporous channels can be formed after in-situ hydrolysis, and the diffusion efficiency of a product is improved; and a staged crystallization procedure is adopted, so that rich mesopores among particles and excellent uniformity are ensured.

The invention belongs to the technical field of catalysts, and discloses a preparation method of a water-resistant multi-metal composite catalyst and application of the water-resistant multi-metal composite catalyst in preparation of polyether amine. The preparation method comprises the following steps: (1) mixing a nickel source, a lanthanum source, a chromium source and an aluminum source, adding a precipitant to carry out a co-precipitation reaction, and then aging and granulating to prepare metal hydroxide precipitation particles; and (2) dipping the metal hydroxide precipitation particles into a noble metal precursor solution, then roasting, processing and forming, and finally reducing to obtain the multi-metal composite catalyst. By optimizing the preparation process, high-dispersion noble metal active sites are formed, the catalytic activity and water resistance of the catalyst in hydroamination reaction can be effectively improved, and the cost is reduced. When being applied to synthesis of polyether amine, the catalyst can effectively resist the influence of water generated in synthesis reaction of polyether amine on the catalyst, prolong the service life of the catalyst and ensure long-term stable operation of the catalyst in actual production.

The invention relates to a synthesis method of 1H-pyrrolo [3, 2-B] pyridine-6-amine. Comprising the following steps: carrying out a reaction on 5-bromo-2-methyl-3-nitropyridine and N, N-dimethyl formamide dimethyl acetal to obtain (E)-2-(5-bromo-3-nitropyridine-2-yl)-N, N-dimethyl ethylene-1-amine, and carrying out a reaction on the (E)-2-(5-bromo-3-nitropyridine-2-yl)-N, N-dimethyl ethylene-1-amine and the N, N-dimethyl formamide dimethyl acetal to obtain the 5-bromo-2-methyl-3-nitropyridine. Adding the 6-bromine-4-azaindole into acetic acid, and performing reduction and cyclization reaction by using an iron-based catalyst to obtain 6-bromine-4-azaindole; and then adding into ammonia water, and reacting under a copper-based catalyst to obtain the 1H-pyrrolo [3, 2-B] pyridine-6-amine. The 1H-pyrrolo [3, 2-B] pyridine-6-amine is effectively obtained through three-step synthesis. A compound of Fe-coated PMMA-b-PDMAEMA and PE wax coated iron powder is used as an iron-based catalyst, and the ratio of the Fe-coated PMMA-b-PDMAEMA to the PE wax coated iron powder is reasonably adjusted, so that the catalytic effect of the reduction and cyclization reaction is remarkably improved and further optimized, and the conversion rate is improved, thereby realizing high yield of the product.

The wisdom utilization of nuclear energy plays a core and irreplaceable role in consolidating national defense security and transforming energy system to green. While the nuclear energy technology is booming, how to properly manage and efficiently resource the depleted uranium (especially 238 U, although it does not constitute direct radioactive hazard to human body) generated in the process of nuclear energy application has become an urgent and key technical challenge in the field of environmental protection and sustainable development. In particular, we use U3O8 prepared from depleted UF6 as raw material, and use UO4·2H2O prepared by simple dissolution and precipitation as catalyst to catalyze the synthesis of diphenyldiazene or its derivatives from aniline: one aspect of the invention creates a way to reuse depleted uranium waste, finding a new way to transform this traditionally difficult waste, and on the other hand, it ingeniously builds a bridge from aniline and its derivatives to high value-added chemicals-diphenyldiazene or its derivatives. Not only can it effectively reduce the potential threat of depleted uranium waste to the environment, realize the green transformation and resource utilization of waste, but also can promote the chemical industry to a more efficient and environmentally friendly direction, and bring significant economic benefits to the chemical industry.

The utility model relates to the technical field of mesosulfuron-methyl synthesis, and particularly discloses a mesosulfuron-methyl nitration reaction device, which comprises a reaction kettle, a feed inlet and a waste gas outlet are arranged on the top of the reaction kettle, a discharge port is arranged at the bottom of the reaction kettle, and a detachable sealing cover is installed on the discharge port through a threaded connection mode; a spiral propelling type stirrer is vertically arranged in the reaction kettle, the spiral propelling type stirrer comprises a stirring shaft and spiral blades that are continuously distributed along the stirring shaft from top to bottom, the distance between the outer edge of the spiral blade and the inner wall of the reaction kettle is 5-8 mm, a polytetrafluoroethylene coating with a thickness of 0.2-0.5 mm is coated on the surface of the spiral blade, and a motor is coaxially and fixedly connected to the driving stirring shaft on the top of the reaction kettle; through the cooperation of the spiral propelling type stirrer and the polytetrafluoroethylene coating, the gradient temperature control of the multi-stage variable-diameter cooling coil, the precise distribution of the 40-degree inclined atomizing nozzle, and the synergistic design of the pH closed-loop discharge control, the nitration reaction efficiency and the product purity are significantly improved.

The application discloses a method for synthesizing diphenylamine from aniline. μ -H)3IrCp*][X] (Cp*: pentamethylcyclopentadiene; X: BF4 — , PF6 — , BPh4 — , CF3SO3 — ) as a catalyst, and diphenylamine is obtained under the conditions of a reaction temperature of 100-300 DEG C and a reaction pressure of 0.5-4.0 MPa. The method has high aniline conversion rate and good diphenylamine selectivity, and the catalyst can be recovered through solvent polarity adjustment after the reaction is completed.

The application provides a synthesis method of flumioxazin, and belongs to the technical field of pesticide synthesis. The application takes 2,4-difluoro nitrobenzene as a starting material, and obtains the product flumioxazin through hydrolysis, bromination, etherification, ring closure, propynylization and acylation. The method provided by the application solves the problems of complicated synthesis process, serious environmental pollution and low yield of flumioxazin, and the synthesis method of flumioxazin is suitable for industrial production.

The invention discloses a regeneration liquid of a diphenylamine catalyst synthesized from aniline. The regeneration liquid is prepared from the following components in parts by mole: 15 to 65 parts of N, N-dimethylformamide, 10 to 30 parts of tetrahydrofuran, 10 to 40 parts of N-methyl pyrrolidone and 10 to 60 parts of n-decane. The regeneration liquid provided by the invention can effectively soften and dissolve carbon deposits generated at the initial stage in the process of synthesizing diphenylamine from aniline, especially polyaniline-like carbon deposits, and coke carried outside the polyaniline carbon deposits and further generated falls off together, so that the catalyst can be thoroughly decarbonized to obtain a better regeneration effect.

A triethylenetetramine synthesis system, relating to the field of triethylenetetramine production technology, includes an amination reactor, a circulating gas heater, a product collection tank, a liquid-phase mixture separation mechanism, and a gas-phase mixture separation mechanism. The amination reactor has a gas inlet and a liquid outlet at its top and bottom, respectively, and a liquid inlet and a gas outlet on its upper and lower outer walls, respectively. The liquid-phase mixture separation mechanism is connected to the liquid outlet, the gas-phase mixture separation mechanism, the product collection tank, and the cold fluid inlet of the circulating gas heater. The gas-phase mixture separation mechanism is connected to the gas outlet and the cold fluid inlet of the circulating gas heater. The cold fluid outlet of the circulating gas heater is connected to the gas inlet. This invention solves the problem of high circulating gas and product loss rates in existing triethylenetetramine synthesis systems.

The invention relates to the technical field of tropicamide synthesis mother liquor recovery, and provides a tropicamide synthesis mother liquor recovery system and method.The system comprises a pH stirring and adjusting tank body, a filter box, a mounting frame, a filter bag, a fine filter screen, a first driving motor, an adapter plate, a sliding connection sleeve plate, a deslagging door and a top plate. The filter box body is arranged to be a rectangular box body, assembly of a rectangular mounting frame is facilitated, meanwhile, a first driving motor can conveniently adjust the mounting frame to rotate, and the mounting frame is arranged to be rotatable, so that when impurities attached to a filter bag need to be cleaned, the mounting frame is adjusted to rotate; the filter bag is arranged in the mounting frame, the filter surface of the filter bag is ejected out of the mounting frame through the top plate, flushing water flowing through the flowing channel can flush the surface of the filter bag, and the fine filter screen can be rotated to be inclined through the rotationally arranged adapter plate, so that the filter bag and the fine filter screen do not need to be disassembled; therefore, impurities attached to the filter bag and the fine filter screen can be cleaned, and the device is convenient to use.

The invention provides a pyrimidine and selenide-containing pincerlike N-heterocyclic carbene (NCSe pincerlike NHC) palladium complex as well as a preparation method and application thereof, belongs to the technical field of organic synthesis and metal complex catalysis, and aims at solving the technical problems of low catalyst efficiency, narrow substrate application range, oxidant dependence and the like in photocatalytic amide synthesis. The NCSe pincerlike NHC palladium complex has a structural general formula shown in the specification. The NCSe pincerlike NHC palladium complex is prepared by the following steps: reacting a chlorinated imidazole derivative with alkyl sodium selenol to obtain a selenide functionalized imidazole derivative intermediate, then carrying out an ionization reaction on the selenide functionalized imidazole derivative intermediate and 2-halogenated pyrimidine to obtain N, N '-pyrimidine and selenide disubstituted imidazolium salt, and finally reacting with a palladium source under an alkaline condition to obtain the target product NCSe pincerlike NHC palladium complex. The NCSe pincerlike NHC palladium complex can efficiently catalyze the direct oxidative coupling reaction of aromatic aldehyde and secondary amine, no stoichiometric oxidant is needed, and a series of tertiary amide products are synthesized at high yield. The method has the advantages of mild and green reaction conditions, wide substrate universality, simple and practical operation, and good application prospects.