26results about "Hydrazine preparation" patented technology

The invention discloses a preparation method of an omariglone key intermediate, which comprises the following steps: under the common catalytic action of a catalyst and a ligand, taking 4-bromo-2, 6-dimethyl fluorobenzene and hydrazine hydrate as initial raw materials, adding an additive and a solvent, and synthesizing the omariglone key intermediate under a heating condition. The preparation method provided by the invention is simple to operate, mild in reaction condition and high in atom economy, the synthesis cost is reduced, and industrial-grade large-scale production is realized.

The present application relates to the technical fields of reaction kettle, and discloses a reaction kettle for preparing methylhydrazine aqueous solution, which comprises a reaction kettle, a rotating shaft arranged in the reaction kettle, an end cover arranged at the top end of the reaction kettle, a stirring frame arranged on the rotating shaft, the stirring frame comprising an upper cross beam, a lower cross beam and a connecting rod, the two ends of the connecting rod being connected with the upper cross beam and the lower cross beam respectively, a conveying belt arranged on the stirring frame, the conveying belt being rotatably arranged on the stirring frame, a first driving mechanism arranged on the stirring frame and used for driving the conveying belt to rotate, a discharge chute arranged on the side wall of the rotating shaft, the side of the conveying belt being abutted against the side wall of the discharge chute, the other side of the conveying belt having a gap with the side wall of the discharge chute, the rotating shaft being a hollow shaft, a screw blade being arranged in the rotating shaft, a liquid passage being arranged on the rotating shaft close to the bottom of the reaction kettle, and a discharge port being arranged at the bottom end of the reaction kettle; the reaction kettle for preparing methylhydrazine aqueous solution can separate the catalyst from the liquid after reaction.

This invention relates to the field of pharmaceutical impurity preparation technology, and discloses a method for synthesizing apixaban genotoxic impurity I. The steps include: S1. performing an addition reaction of compound II in an alkaline system to generate compound III; S2. subjecting the product of S1 to elimination and isomerization reactions under heating, separating the reaction product to obtain apixaban genotoxic impurity I. The synthesis method of this invention has high safety, low raw material cost, and can achieve a one-pot reaction while ensuring yield and product purity (no product separation and purification is required between each reaction step; only one separation and purification is needed after obtaining the final product).

This invention relates to the field of biomaterial synthesis technology, specifically disclosing a method for preparing a class of catechol derivatives and their applications, administration, and preparation apparatus. The methods include: preparing dopa or carbidopa derivatives using a sodium sulfite-boric acid-argon protective system in an organic-aqueous mixture; or using dopa as a raw material, performing a methyl esterification reaction with SOCl2 and anhydrous methanol, followed by an exchange reaction with methyl trifluoroacetate to achieve a one-pot synthesis of Tfa-DOPA-OMe; or preparing acetal-protected tanshinone derivatives based on dopa derivatives or tanshinone and its derivatives; or using acetal-protected tanshinone and its esters to prepare natural catechol compounds such as Shimobashiric acid C, and preparing non-natural catechol compounds through coupling reactions with organic acids, amino acids and their derivatives, oligopeptides and polypeptides, alcohols, or sugars. Highly selective deprotection conditions achieve the goal of completely and thoroughly removing the acetal protection of catechols without destroying the ester bonds within the molecular structure.

The invention discloses a preparation method of a cerium oxide supported palladium catalyst and application of the cerium oxide supported palladium catalyst in catalytic hydrogenation of azo compounds. According to the catalyst, nano octahedral cerium oxide serves as a carrier, palladium is loaded through an impregnation method, and a high-dispersion Pd / CeO catalytic system is formed. The octahedron of cerium oxide and the hydrogenation activity of palladium have a synergistic effect, the hydrogenation efficiency and selectivity of the catalyst are remarkably improved, the catalyst is suitable for hydrogenation reduction reaction of hydrogenated azo compounds, the preparation method of the catalyst is simple, the cost is low, the hydrogenated azo compounds can be efficiently catalyzed under mild conditions, and compared with a traditional Pd / C catalyst, the catalyst has good application prospects. The catalyst has higher activity and stability.

The invention provides a preparation method of a prothioconazole intermediate, which comprises the following steps: (1) reacting a hydrazino substance with formaldehyde under an alkaline condition to obtain an intermediate product, and (2) reacting the intermediate product, thiocyanate and a polymerization inhibitor under an acidic condition to obtain the prothioconazole intermediate, the structural formula of the intermediate is as follows: the polymerization inhibitor is selected from one or more of a phenol polymerization inhibitor and an inorganic salt polymerization inhibitor. The intermediate prepared by the preparation method provided by the invention has higher purity and yield, and is simple to operate and especially suitable for industrial production.

The invention discloses a methylhydrazine continuous flow synthesis process based on coupling of a microchannel reactor and a tubular reactor, and relates to the technical field of chemical engineering. The method comprises the following steps: by taking hydrazine hydrate, hydrochloric acid and methanol as raw materials, continuously introducing the raw materials into a micro-channel reactor through a metering pump to realize rapid mixing, preheating and preliminary methylation reaction so as to generate a reactant flow containing methylhydrazine hydrochloride; introducing the material flow into a series tubular reactor, carrying out constant-temperature and constant-pressure curing reaction, and prolonging the retention time so as to improve the conversion rate; and carrying out continuous dissociation and rectification separation to obtain a high-purity methylhydrazine product. The process overcomes potential safety hazards and efficiency limitation of traditional intermittent kettle reaction, enhances heat and mass transfer, improves reaction controllability and industrial applicability, and is suitable for continuous production of high-heat-release and high-risk methylation reaction.

The utility model discloses a recycling device for mother liquor in carbazide production, and relates to the technical field of carbazide production, an inlet of a distillation kettle is communicated with a mother liquor tank, an outlet of the distillation kettle is communicated with a crystallizing tank through a pipeline, and an outlet of the crystallizing tank is communicated with a first centrifugal machine; and a solid phase outlet of the first centrifugal machine is communicated with a hydrazine crystal tank. The mother liquor is distilled by the distillation kettle, and moisture and low-boiling-point impurities in the mother liquor are evaporated by heating, so that primary concentration and component separation of the mother liquor are realized, and a proper concentration condition is created for subsequent crystallization. And the concentrated mother liquor in the crystallizing tank is cooled and the like, and the carbazide reaches a supersaturated state so as to be crystallized and separated out. The first centrifugal machine is used for separating carbazide crystals formed in the crystallizing tank from mother liquor, and the solid phase outlet is connected with the carbazide crystal tank, so that the carbazide crystals are preliminarily recovered, the whole process is coherent, and basic operation from mother liquor to preliminary recovery of the carbazide crystals is reasonably realized.

The invention discloses a diaryl hydrazine compound and a preparation method thereof, and the preparation method comprises the following steps: mixing an azobenzene compound, an alkyl NHPI ester reagent, a photosensitizer, an alkaline reagent and a solvent, and reacting under the irradiation of visible light to obtain the diaryl hydrazine compound, wherein the photosensitizer is one or a mixture of two of 2, 4, 5, 6-tetrakis (carbazole-9-yl)-1, 3-dicyanobenzene, di [2-(2, 4-difluorophenyl)-5-trifluoromethylpyridine] [2-2 '-bis (4-tert-butylpyridine)] iridium hexafluorophosphate, and the solvent is one or a mixture of two of 2, 4, 5, 6-tetrakis (carbazole-9-yl)-1, 3-dicyanobenzene and di [2-(2, 4-difluorophenyl)-5-trifluoromethylpyridine] [2-2'-bis ( And the alkaline reagent is one or a mixture of more of N, N-diisopropylethylamine, potassium phosphate and 1, 8-diazabicyclo [5.4. 0] undec-7-ene. The preparation method disclosed by the invention has the advantages of easily available raw materials, simplicity in operation, mild reaction, wide substrate applicability and the like.

The invention discloses a high-enthalpy-value metal-organic coordination material as well as preparation and application thereof, and belongs to the field of phase change energy storage. According to the metal-organic coordination material, transition metal nitrate is coordinated with acethydrazide in a small molecule amide ligand to obtain a series of metal-organic coordination materials. The material realizes the synergistic effect of a hydrogen bond network and a metal coordination bond, so that the material has the advantages of high phase change temperature, large enthalpy value and the like. Compared with a traditional phase change material, the phase change material has excellent thermodynamic property and thermal stability. The device can be applied to the field of heat management of high-power equipment, has the advantages of high energy storage density, low material consumption and the like, and has wide application prospects.

The application discloses a preparation method of arylhydrazine compounds. The preparation method of the arylhydrazine compounds comprises the following steps: mixing a mixed metal catalyst, a thiourea compound, a compound of formula I and a compound of formula II under alkaline conditions to obtain a mixture, and performing reaction to obtain the arylhydrazine compounds. The general formula of the compound of formula I is as follows: the general formula of the compound of formula II is as follows: R 2 NHNH2. The preparation method can synthesize the arylhydrazine compounds in one step, the preparation method can select inexpensive and easily obtained catalysts and raw materials, the preparation method has good selectivity, is non-toxic, has high yield, is low in cost and is convenient for large-scale preparation.

The invention relates to the technical field of reaction kettles, and particularly discloses a reaction kettle for preparing a methylhydrazine aqueous solution, which comprises a reaction kettle, a rotating shaft arranged in the reaction kettle, an end cover arranged at the top end of the reaction kettle, a stirring frame arranged on the rotating shaft, the stirring frame comprises an upper cross beam, a lower cross beam and a connecting rod, and two ends of the connecting rod are respectively connected with the upper cross beam and the lower cross beam. A conveying belt is arranged on the stirring frame and rotationally matched with the stirring frame, a first driving mechanism is arranged on the stirring frame and used for driving the conveying belt to rotate, a discharging groove is formed in the side wall of the rotating shaft, one side of the conveying belt abuts against the side wall of the discharging groove, a gap is formed between the other side of the conveying belt and the side wall of the discharging groove, and the rotating shaft is a hollow shaft. A liquid through hole is formed in the rotating shaft close to the bottom of the reaction kettle, and a discharge hole is formed in the bottom end of the reaction kettle; the reaction kettle for preparing the methylhydrazine aqueous solution can separate a catalyst from reacted liquid.

The invention discloses a continuous catalysis system and method for synthesizing methylhydrazine, and relates to the technical field of methylhydrazine synthesis. Comprising the following steps: mixing hydrazine hydrochloride with pure water, heating in a water bath, and stirring until solids are completely dissolved to form a clear and transparent solution to obtain a methanol catalytic solution; the hydrazine hydrochloride raw material liquid and the methanol catalytic liquid are synchronously conveyed to a continuous reaction device with a microchannel connected with a subsequent reaction section in series, and a continuous catalytic alkylation reaction is completed; the method comprises the following steps: removing methanol from reaction discharge liquid through normal-pressure distillation, recovering, adding caustic soda liquid into residual liquid, stirring, standing for layering, taking an organic phase, carrying out reduced-pressure rectification, collecting a target fraction to obtain a methylhydrazine product, and carrying out gradient heating and precise pressure regulating technologies to realize stable control of reaction pressure. The small-volume continuous flow design is used for replacing the traditional large-volume intermittent kettle reaction, so that the core problems of prominent high-pressure risk and high danger coefficient of the traditional process are solved, and the intrinsic safety level of methylhydrazine synthesis is improved.

The invention discloses a synthesis method of high-selectivity trimethylhydrazine, which comprises the following steps: preparing a catalyst: loading Al < 3 + > by using UiO-AI as a carrier through a dipping-roasting method to obtain a UiO-AI catalyst; the method comprises the following steps: constructing a reaction system: dissolving hydrazine hydrochloride in gamma-valerolactone to prepare a raw material solution, and preparing a methylation reagent solution from biomass methanol and deionized water; regulating and controlling micro-channel reaction: pumping the raw material solution and the methylation reagent solution into a micro-channel reactor, and regulating and controlling reaction parameters in real time by an LSTM module; post-treatment: filtering and recovering the catalyst, adding KOH into the filtrate for dissociation, extracting with ethyl acetate, carrying out reduced pressure rectification, and collecting a fraction at 88-90 DEG C to obtain trimethylhydrazine with the purity of more than or equal to 99.5% and the yield of more than or equal to 90%. According to the method, the traditional pain point of trimethylhydrazine synthesis can be solved, the blank of high-quality production of optical pure derivatives in China can be filled up, the medical intermediate industry is promoted to be transformed to be high-efficiency, green and high-end, and the method has remarkable technical value and economic significance.

Aspects of the present application relates to solid state forms of Pirtobrutinib such as novel crystalline form P1, amorphous solid dispersions comprising Pirtobrutinib and pharmaceutically acceptable carriers and processes thereof, wherein the pharmaceutically acceptable carrier is selected from the group consisting of HPMC phthalate, HPC, Eudragit L100, microcrystalline cellulose, carboxymethyl cellulose, mannitol, Neusilin, cellulose acetate phthalate, polyvinyl alcohol, polylactic-co-glycolic acid, polyvinyl acetate phthalate, sodium alginate, beta cyclodextrin, and mixtures thereof. Aspects of the present application relates to process for the preparation of [(1S)-2,2,2-trifluoro-l-methyl- ethyl]hydrazine or its salts.

The invention relates to a method for preparing hydrazine hydrate, which comprises the following successive steps: a) preparing, by means of an absorption column, an aqueous solution containing solubilised ammonia and containing at least one activator, by introducing an aqueous solution comprising at least one activator and fresh ammonia into the absorption column; then b) reacting, inside at least one reactor, the aqueous ammonia solution containing at least one activator obtained in the preceding step with hydrogen peroxide and a ketone; then c) separating the azine-containing organic phase of the aqueous phase from the stream formed as a result of the preceding step; and then d) hydrolysing the organic phase obtained in the previous step to obtain hydrazine hydrate.

The invention relates to a novel method for synthesizing arylhydrazine, which is characterized in that arylhydrazine sulfonate is subjected to catalytic hydrogenation to obtain arylhydrazine, the used catalyst is a supported noble metal catalyst, and the catalytic hydrogenation method comprises the following steps: adjusting the pH value of an arylhydrazine sulfonate solution to be greater than or equal to 12; and heating the solution, maintaining the temperature of the solution at 30-120 DEG C, adding a catalyst into the solution, introducing hydrogen until the solution does not absorb hydrogen any more, cooling, and filtering to remove the catalyst, thereby obtaining the aryl hydrazine solution. The arylhydrazine prepared by catalytic hydrogenation of the arylhydrazine sulfonate can be obtained by only one step, two steps of removing sulfonate groups by hydrochloric acid and neutralizing are not needed, the synthesis efficiency is improved, the yield is improved, and the three wastes are greatly reduced.

The application discloses a method for selectively preparing azoxybenzene or 1,2-diphenylhydrazine by hydrogenation of nitrobenzene, which comprises the following steps: adding an oligolayer graphene wrapped Ni catalyst, an alkali, nitrobenzene and a solvent into a polytetrafluoroethylene lining, uniformly mixing by ultrasonic and then sealing into a reaction kettle, replacing the air in the reaction kettle with hydrogen, controlling the temperature to 15-30 DEG C to prepare azoxybenzene, or increasing the temperature to 50-80 DEG C to prepare 1,2-diphenylhydrazine. The oligolayer graphene wrapped Ni catalyst is applied to catalyze the hydrogenation of nitrobenzene to prepare azoxybenzene. The catalyst has the advantages of simple synthesis route, cheap and easily available raw materials, simple reaction condition, easy operation, cheap and easily available nitrobenzene and high economic benefit. The obtained oligolayer graphene wrapped Ni catalyst has the advantages of mild reaction condition, high selectivity to products, easy separation and recovery and good cycle stability in the preparation of azoxybenzene or 1,2-diphenylhydrazine by hydrogenation of nitrobenzene.

This invention discloses a method for synthesizing 4-fluoro-3,5-dimethylphenylhydrazine hydrochloride, belonging to the field of pharmaceutical intermediate synthesis technology. The synthesis method involves the following steps: copper halide, hydrazine additives acting as catalysts, a phase transfer catalyst, K3PO4, and 4-fluoro-3,5-dimethylbromobenzene are added to a solvent, and the temperature is raised to 80℃-100℃; hydrazine hydrate is added dropwise to the above mixture, and after the addition is complete, the temperature is maintained at 80℃-100℃ for 6-10 hours; after the reaction is complete, the temperature is lowered to room temperature, dichloromethane is added, the mixture is filtered, and the filtrate is separated, the aqueous layer is removed, and the organic layer is washed with saturated brine; the washed organic phase is acidified to pH 2-3 to obtain crude 4-fluoro-3,5-dimethylphenylhydrazine hydrochloride; the crude product is recrystallized to remove impurities, yielding a finished product with a purity of over 99%. This invention utilizes readily available raw materials, achieves high yield, produces a high-purity finished product, has a simple preparation method, a short processing cycle, and low manufacturing cost.

The invention belongs to the technical field of preparation of oxadiazon intermediates, and particularly discloses a method for continuously preparing 2, 4-dichloro-5-isopropoxy phenylhydrazine hydrochloride. The method comprises the following steps: respectively precooling a 2, 4-dichloro-5-isopropoxy chlorobenzene diazonium salt solution and a stannous chloride aqueous solution, introducing into a microchannel reactor after precooling, mixing, and reacting to obtain the 2, 4-dichloro-5-isopropoxy phenylhydrazine hydrochloride. The mixing effect of the diazonium salt and the reducing agent stannous chloride is enhanced by utilizing a micro-reaction technology, the reaction speed is increased, the mass transfer and heat transfer effects are improved, and the problems of poor heat and mass transfer effects, low production efficiency, uncontrollable reaction process and accumulation of a large amount of diazonium salt in the existing intermittent reaction are solved; and the existing continuous reaction has the problems of high cost and poor stability.

The invention belongs to the field of jet fuel thermal oxidation inhibition, and particularly relates to a hydrazine compound, a hydrazine composite material, a preparation method thereof and application of the hydrazine compound and the hydrazine composite material in jet fuel efficient deoxidation. The hydrazine compound and the hydrazine composite material are successfully prepared as the jet fuel deoxidant. The hydrazine compound is prepared by adopting an alkali washing method, and the hydrazine composite material is prepared by mixing and dispersing the porous carrier and a hydrazine compound solution, performing rotary evaporation to remove a solvent and drying. The hydrazine composite material can reduce the dissolved oxygen content of the jet fuel to 1 ppm or below, and the thermal oxidation deposition amount is reduced by 90%.

The invention discloses a gossypol derivative, a preparation method thereof and application of the gossypol derivative in preparation of a coronavirus 3CL protease inhibitor, and belongs to the field of medical chemistry. The novel gossypol derivative is obtained by carrying out structural modification on gossypol by utilizing isocyanate or a primary amine compound. Preliminary tests show that the gossypol derivative obtained by the method can effectively block RNA (Ribonucleic Acid) replication and transcription processes by inhibiting 3CLpro so as to block virus proliferation, exert an anti-coronavirus effect and remarkably reduce the activity of 3CLpro protease, is long in acting time, strong in drug effect and not easy to generate drug resistance, can be used for preventing and treating coronavirus infection, and has a good application prospect. Therefore, the compound can be used for preparing medicines for preventing, treating and diagnosing coronavirus.

The application belongs to the field of pharmaceutical chemical industry, and particularly relates to a production method of a key intermediate of alamorelin, i.e. trimethylhydrazine hydrochloride. The technical scheme of the application comprises the following steps: step 1. synthesis of compound 2 is divided into two stages: stage 1. under the action of an alkali, hydrazine formic acid tert-butyl ester is reacted with a methylating agent to generate a mixture of compound 3 and compound 2. The mixture does not need to be further purified and separated, and is directly used in the second stage; stage 2. the mixture in the above step is further reacted with the methylating agent to be completely converted into compound 2, and step 2. compound 2 is removed from Boc protection in the presence of hydrochloric acid, and is salified to obtain trimethylhydrazine hydrochloride. The application provides a preparation method of trimethylhydrazine hydrochloride suitable for industrial production, and solves the problems of high production cost and safety hazards existing in the prior art.

The present invention provides conjugates comprising a sugar such as mannitol and one or more L-DOPA and / or DOPA decarboxylse inhibitors including, inter alia, L-DOPA, carbidopa, benserazide, or a combination thereof, wherein the sugar is conjugated to the carboxyl group of the L-DOPA and / or DOPA decarboxylse inhibitor / s) via a hydroxyl group of the sugar. The present invention further provides related pharmaceutical compositions and methods of producing the conjugates, as well as methods of use for treating medical disorders responsive to dopamininergic stimulation such as movement disorders including, inter alia, Parkinson's Disease.

The application relates to a reducing carrier loaded metal nanoparticle and its application in preparation of azoarenes, relates to the field of catalytic hydrogenation of nitroarenes, and is characterized in that the reducing carrier loaded metal nanoparticle is dispersed into an alcohol solvent containing a bidentate amine assistant, a nitroarene is added, air in a reaction container is discharged by introducing hydrogen, hydrogen with a pressure of 0.1-0.6 MPa is kept, a catalytic hydrogenation reaction is carried out below 5 DEG C, after the hydrogenation reaction is completed, air is introduced into the reaction container to carry out an oxidation reaction, and azobenzene (I) is obtained, wherein R is selected from hydrogen, an alkyl group, halogen, an alkoxy group, a hydroxyl group, an amino group or an acyl group.