143 results about "Salt formation" patented technology

The invention provides a chiral resolution method and application of a 3-aryl substituted glutaric acid monoester compound, and the method comprises the following steps: taking a substance as shown in a formula I as a starting raw material, and carrying out alcoholysis to obtain a racemic intermediate as shown in a formula IV; and splitting the intermediate shown in the formula IV, and then dissociating to obtain the compound shown in the formula III, which has a single spatial configuration and an ee value of more than 99%. A cyclic anhydride substrate with a symmetrical structure is used and reacts with alcohol to obtain racemic 3-aryl substituted glutaric acid monoester, a target configuration with high chiral purity is obtained by screening some resolution reagents and solvents and performing salifying resolution on the 3-aryl substituted glutaric acid monoester, the operation is simple, the resolution reagents are easily available in the market and can be recycled, and the method is suitable for industrial production. The method has the advantages that an expensive chiral catalyst or a harsh enzyme catalysis condition is avoided, the reaction cost is reduced, amplified production is facilitated, the ee value of a target configuration can be increased to 99% or above, and the method is an economic and environment-friendly technical route which is simple in post-treatment and convenient for amplified production.

A preparation equipment and a process for a nylon salt solution. The preparation equipment includes a suspension preparation device, a first salt formation reactor and a second salt formation reactor. The suspension preparation device includes a feeding unit, a continuous feeding unit, a high-shear pump and a mixing reactor, the high-shear pump and the mixing reactor are cyclically connected with and in communication with each other through two connecting pipelines; the second salt formation reactor includes a second diamine feed pipe, a third diamine feed pipe, a circulation pipeline of the second salt formation reactor and an online near-infrared monitoring equipment located on the circulation pipeline of the second salt formation reactor.

The invention discloses a preparation method of 3-quinuclidinone hydrochloride, which comprises the following steps: carrying out temperature control reaction on 4-picolinic acid and chloroacetic acid under alkaline water conditions to obtain an aqueous solution of a compound a, and directly entering the next reaction without post-treatment after the reaction is finished; adding a reducing agent alkaline water system into the aqueous solution of the compound a, controlling the temperature to react, controlling the temperature to adjust the pH value to 5-5.5 after the reaction is finished, extracting with n-butyl alcohol, and drying to obtain an n-butyl alcohol solution of a compound b, and directly entering the next reaction step; wherein the reducing agent is one of sodium borohydride and potassium borohydride; dropwise adding thionyl chloride into an n-butyl alcohol solution of the compound b, controlling the temperature to react after dropwise adding is ended, and concentrating to remove the solvent and unreacted thionyl chloride after the reaction is ended, so as to obtain a compound c; carrying out Dieckmann condensation reaction on the compound c at controlled temperature under the condition of organic alkali by using toluene as a solvent, carrying out hydrochloric acid quenching reaction after the reaction is finished, and directly carrying out next-step reaction after extracting and removing impurities from a water phase containing a hydrochloride solution of a compound d by using toluene; and carrying out a decarboxylation reaction on the compound d in a hydrochloric acid aqueous solution at controlled temperature, after the reaction is finished, adjusting the pH value to 10-13, extracting, and salifying to obtain a target compound TM, namely 3-quinuclidinone hydrochloride. The preparation method of 3-quinuclidinone hydrochloride provided by the invention has the advantages of economical and easily available raw materials, mild reaction conditions, efficient reaction, simple operation and low cost, and is suitable for industrial application.

The present invention provides a DIDNTB alkali metal salt, a preparation method and an application thereof, belonging to the technical field of DIDNTB salt formation. The DIDNTB alkali metal salt described in the present invention is a DIDNTB lithium salt, a DIDNTB sodium salt and a DIDNTB potassium salt. The preparation method of the present invention is as follows: Mix DIDNTB and an alkali metal salt in a solvent for a salt formation reaction to obtain a crude DIDNTB alkali metal salt; Mix the crude DIDNTB alkali metal salt with a solvent for recrystallization to obtain the DIDNTB alkali metal salt. The DIDNTB alkali metal salt obtained in the present invention overcomes the deficiency of poor water solubility of the existing DIDNTB, and the preparation process method is simple, the conditions are mild, the product purity is high, the yield is high, the cost is low, and it can be mass-produced, which is beneficial to further application in detection reagents.

The present invention provides a method for separating and purifying mevastatin from a mevastatin mother liquor. The method primarily comprises the steps of gradient hydrolysis ring-opening and salt formation, stripping and impurity removal, extraction and purification, and condensation ring-closure. The gradient hydrolysis ring-opening step controls the generation of impurities, and this, combined with the stripping and impurity removal step, synergistically improves the yield and purity of mevastatin. The mevastatin separation and purification method provided by the present invention ultimately yields mevastatin with a purity exceeding 90% and a yield exceeding 80%.

The application belongs to the technical field of pharmaceutical chemistry synthesis, and specifically discloses a preparation method of oseltamivir and a phosphate thereof and an intermediate thereof, which comprises the following steps: (1) a compound of formula VII is reacted with VIII under the action of a base in a solvent to obtain an intermediate of formula VI, and then the intermediate of formula VI is reacted under the action of a strong base at high temperature to obtain formula V; (2) formula V is subjected to ring-opening reaction with tert-butylamine in a solvent under the catalysis of a Lewis acid to obtain formula IV; (3) formula IV is reacted with an acetylating agent in a solvent under the action of a base to obtain formula III; (4) formula III is reacted under the action of an acid at a certain temperature to obtain formula II; and (5) formula II is subjected to salt formation with phosphoric acid in a solvent to obtain oseltamivir. The preparation method has the characteristics of simple operation, low cost, high yield, high optical purity of the product, stable process and the like, and is suitable for industrial production.

This invention relates to the field of pharmaceutical technology and discloses a method for improving the clarity and color of oxybuprocaine hydrochloride solution, comprising the following steps: S110: Oxoplasmin is added to a reactor, and an organic solvent is added while stirring to control the reaction system at 0-10°C; an antioxidant is added. S120: Hydrochloric acid is slowly added in batches to the temperature-controlled reaction system. After the addition is complete, the temperature is controlled at 0-10°C for 2-4 hours, then the temperature is raised to 40-50°C for 2-4 hours, and activated carbon is added. S130: The mixture is filtered while hot, and solvent is slowly added dropwise to the filtrate until the product precipitates. After slurrying at 25-35°C for 2 hours, the mixture is filtered, and the filter cake is vacuum dried in a vacuum drying oven at 40-50°C for 12-16 hours to obtain oxybuprocaine hydrochloride. This invention provides a novel method for obtaining oxybuprocaine hydrochloride by adding antioxidants and activated carbon in the salt formation step. The clarity and color of the resulting product solution meet pharmacopoeia requirements.

The invention belongs to the technical field of drug synthesis, and particularly relates to a beraprost sodium preparation method, which comprises: (1) adding beraprost into a methanol solution, and adding a sodium hydroxide aqueous solution to carry out a reaction to form a salt; (2) after salifying, concentrating under reduced pressure, and adding an organic solvent for concentrating again; and (3) after the concentration is finished, adding an organic solvent, heating and dissolving, then slowly cooling to 0-5 DEG C, crystallizing, filtering and drying to obtain the beraprost sodium. The synthesis method is simple, convenient to operate, low in cost, high in efficiency, short in production period and suitable for industrial production.

The application discloses a synthesis method of 3,3-difluorocyclopentylamine hydrochloride, and particularly relates to the technical field of chemical synthesis. The synthesis method comprises the following steps: taking 2-cyclopentenone and phthalimide as raw materials, and sequentially performing a Michael addition reaction, deoxygenation fluorination, removal of a phthaloyl protecting group, Boc protection and deprotection and salt formation reaction to obtain 3,3-difluorocyclopentylamine hydrochloride. The synthesis route and process design of the application are reasonable, the starting raw material is 2-cyclopentenone, the required reaction condition is mild, the post-treatment method is simple, the operability is strong, the raw material and reagent are cheap and easy to obtain, and the total yield can reach 43.6%, so the synthesis method has large-scale preparation value.

This invention relates to the field of chemical process technology, specifically to a method for preparing sodium hexafluoroantimonate. The preparation method includes the following steps: (1) adding antimony trioxide, hydrogen fluoride aqueous solution, and sodium fluoride into a reaction vessel, stirring and heating, introducing a fluorine-nitrogen mixed gas, and then refluxing the reaction; (2) filtering and then flash evaporation concentration; (3) subsequently cooling and crystallizing at 0~15℃, and centrifuging to obtain sodium hexafluoroantimonate crystals. The preparation method provided by this invention can achieve fluorination, oxidation, and salt formation in one step simultaneously, with a simple process route and a significant reduction in steps; using low-concentration fluorine gas as an oxidant and fluorine source, the atom utilization rate is high, the reaction rate is fast, the raw material consumption is close to the stoichiometric ratio, the final product has a trivalent antimony residue of ≤0.01%, and the product purity is as high as 99.9%; combined with flash evaporation concentration, hydrogen fluoride and mother liquor recovery and recycling process, it can reduce raw material consumption and waste liquid discharge, thereby improving product yield and reducing production costs.

The invention relates to the technical field of organic synthesis, in particular to a refining method of a crude product of dextroborneol, which comprises the following steps: sequentially carrying out a rearrangement reaction, an esterification reaction, a salt forming reaction, an alkaline hydrolysis reaction and post-treatment refining on the crude product of dextroborneol in the presence of a solvent and a catalyst on the basis of a reaction product to obtain a refined product of dextroborneol, in the refined dextroborneol product, the content of dextroborneol is greater than or equal to 98.0%, the content of L-borneol is less than or equal to 1.0%, the content of isoborneol is less than or equal to 0.15%, the content of natural camphor is less than or equal to 0.15%, and the content of other impurities is less than or equal to 0.10%. The method has the advantages that the isoborneol structure can be selectively destroyed under mild conditions, impurities are effectively removed through the esterification-salification-alkaline hydrolysis three-step reaction, and the purity and yield of dextroborneol are remarkably improved.

The invention belongs to the field of medicinal chemistry, and particularly relates to a preparation method of a lutrombopag intermediate, which comprises the step of preparing an intermediate I p-toluenesulfonate by using a new salifying system.

The application discloses a preparation method of a trans-7H-pyrrolo[2,3-d]pyrimidine compound, and the full name of the trans-7H-pyrrolo[2,3-d]pyrimidine compound is trans-N-methyl-4-(methyl-7H-pyrrolo[2,3-d]pyrimidin-4-ylamino)cyclohexylmethanesulfonamide maleate, which is prepared from trans-4-[(tert-butoxycarbonyl)amino]cyclohexane carboxylic acid and 4-chloro-7H-pyrrolo[2,3-d]pyrimidine as starting materials through reduction, chlorination, substitution, oxidation, methylation, condensation and salt formation reactions. The preparation method has the advantages of few reaction steps, simple operation, low production cost, high production efficiency, high yield, high product purity and suitability for scale-up production.

A method for resolving a phenylalanine derivative of formula (I), and an intermediate. The method comprises: a resolving step comprising using a resolving reagent to react with the phenylalanine derivative represented by formula (I) in a reaction solvent to obtain a resolved intermediate, wherein the resolving reagent is selected from N-acetyl-D-phenylalanine and / or (2R,3R)-(−)-dibenzoyl-L-tartaric acid, and the reaction solvent is selected from 90-99% aqueous ethanol, absolute ethyl alcohol, or acetone. The method uses a chiral reagent to perform salt formation and racemate resolution, and has the advantages of being easy to operate, requiring no special production devices, and being easy to scale up production.

The present invention discloses a preparation method and application of an oxime ester photoinitiator having a donor-acceptor structure. The preparation method constructs a large conjugated donor-acceptor structure oxime ester photoinitiator with triphenylamine as a donor, pyridinium salt as an acceptor, and oxime ester as a photoinitiator group through reactions such as Suzuki coupling, hydroxylation, oxime esterification, and salt formation. The photoinitiator can be used in photocuring systems such as coatings, inks, and 3D printing. It has high photoinitiation efficiency under both visible light and sunlight, and can meet the requirements of deep curing in different complex environments. The photoinitiator has the advantages of high initiation efficiency, ultra-low addition amount, and deep curing depth. The preparation process is simple, the raw materials are easily available, and large-scale industrial production can be achieved.

The present invention belongs to the field of drug synthesis, and in particular to a method for synthesizing oxacillin sodium. The method is based on 6-aminopenicillanic acid (6-APA) and 5-methyl-3-phenyl-4-isoxazolecarbonyl chloride (MPCC) as raw materials, including a synthesis process of a condensation stage, an extraction salt formation stage, and a refined crystallization stage. The method of the present invention adopts a low-temperature phase-splitting process, introduces a phase-transfer catalyst, shortens the reaction time, suppresses the degradation of raw materials, and improves product quality; the refined crystallization stage adopts an inorganic salt-forming agent for refined salt formation, which has lower cost and further reduces the level of impurities. The crystal scale of the product is larger, the product particle size uniformity is better, and the fluidity is better. At the same time, the product does not need to be crushed and can be directly packaged.

The present invention belongs to the technical field of agricultural herbicides and relates to a thiopyralid intermediate compound, a preparation method and an application thereof. The thiopyralid intermediate compound is shown in structural formula (I) and is a stable compound that can be conveniently crystallized, separated, purified, stored and transported. The three-step reaction for preparing the thiopyralid intermediate compound (I) has a stable yield and mild reaction conditions, thereby improving the safety of the process. In addition, in the reaction of synthesizing thiopyralid (II) from the intermediate compound (I) of the present invention, the reaction conditions of the diazotization hydrolysis and salt formation steps are mild, and the yield can reach more than 90%.

The application provides a kind of solvent-free salt formation reaction equipment and process, shell is provided with feed inlet, feed inlet is connected with the grinding chamber in the shell feed, temperature control sleeve is arranged outside the grinding chamber, and the reaction cabin capable of overturning is arranged in the grinding chamber;Ultrasonic tool head is arranged on the grinding chamber above the reaction cabin, the top cover of the reaction cabin can be opened and closed, and the bottom cover of the reaction cabin is hollow fiber reverse osmosis membrane.The process of the application is simple, the combination device can effectively eliminate the influence of raw material residues, the water is removed quickly and completely, the reaction time is short, the energy consumption is low, the content of the obtained product is high, the impurities are few, and a new idea is provided for the synthesis of related products of such raw materials.

The invention provides a preparation method and application of a ziprasidone related substance B, and belongs to the technical field of heterocyclic compound synthesis. Ziprasidone is taken as an object, ziprasidone is salified to synthesize ziprasidone mesylate, ziprasidone mesylate is dissolved and dispersed in a solvent containing activated carbon, after 5-7 days of standing, the solvent is filtered and concentrated, and a related substance B is obtained through crystallization. When the scheme is applied to crystallization of ziprasidone salt, generation of a related substance B can be effectively inhibited, and the product quality is improved.

The application discloses a preparation method of high-purity fluorescein sodium. The fluorescein is synthesized from o-phthalic anhydride and resorcinol under the catalysis of sodium bisulfate or potassium bisulfate without using an organic solvent as a solvent, and then the fluorescein is used to prepare fluorescein diacetate; and the high-purity fluorescein sodium is obtained through a synthesis route of saponification, acidification and salt formation. The synthesis route has mild reaction conditions, simple operation steps, no organic solvent, avoids the generation of organic solvent pollution, has low raw material and auxiliary material consumption, low production cost, high purity of reactants and high yield.

This invention relates to a method for preparing trinitromethyl tricyclic compounds containing nitrogen-rich groups, belonging to the field of energetic materials technology. The specific preparation steps are as follows: Scheme 1 uses 2,3-diaminomaleonitrile to obtain the corresponding methyl ester-substituted intermediate through multiple steps of cyclization, acidification, and esterification. Then, through multiple steps of hydrazine substitution, cyclization with ethyl 3-ethoxy-3-iminopropionate hydrochloride, ester hydrolysis, and nitration, the target compound trinitromethyl tricyclic compound 2 is successfully synthesized. Scheme 2 uses ethyl diazonium acetate to obtain the corresponding methyl ester-substituted intermediate through multiple steps of cyclization, acidification, and esterification. Then, through multiple steps of hydrazine substitution, cyclization with ethyl 3-ethoxy-3-iminopropionate hydrochloride, nitration, salt formation, and renitration, the target compounds trinitromethyl tricyclic compounds 1, 3, and 4 are synthesized. The target compound has advantages such as high nitrogen content, high density, good thermal stability and excellent detonation performance, and can be used as a component of energetic materials, showing potential application value.

This invention discloses a method for synthesizing an intermediate of retinoic acid, relating to the field of pharmaceutical organic synthesis technology, comprising the following steps: S1, in the presence of a base, 2-amino-3-chloropyridine and 4-bromopiperidine undergo a nucleophilic substitution reaction in solvent A to prepare compound III; S2, in the presence of a catalyst and ammonia solution, compound III undergoes an amination reaction in solvent B to prepare compound II; S3, compound II is dissolved in solvent C, and sequentially undergoes CDI cyclization and hydrogen chloride solution salt formation to prepare compound I, namely 1-(piperidin-4-yl)-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one. This invention is low-cost, uses mild reaction conditions, has a simple synthesis process, high yield, and eliminates the need for expensive and potentially unsafe excipients, effectively improving reaction safety, being environmentally friendly, and suitable for industrial production.

The invention discloses a synthesis method of an FLT3 inhibitor of quinatinib dihydrochloride. According to the method disclosed by the invention, the raw material drug of the quinatinib dihydrochloride is synthesized and prepared through seven chemical reactions including Boc protecting group feeding, bromination reaction, condensation ring closing reaction, Boc protecting group removal, phosgene condensation reaction, final etherification reaction to obtain the quinatinib, and final salification. The method has the advantages of wide raw material source, low cost, simplicity in operation, high product recovery rate, easiness in industrial industrialization and the like.

The present disclosure is directed toward a system and a method for storing gas. The system for storing gas comprises a salt formation, an overburden, an underburden, a salt cavern within the salt formation, a sorbent within the salt cavern, and a well traversing the surface that connects the surface with the salt cavern. The method for storing gas comprises several steps. A dissolving fluid comprising water is injected into a salt formation to produce a brine and a salt cavern within the salt formation. The brine is then removed from the salt cavern. A sorbent is then placed within the salt cavern before gas is injected into the salt cavern.

The invention relates to the technical field of preparation of fluorescent materials, in particular to a preparation method of a probe capable of detecting PPi and PFOS, the probe and application. The preparation method comprises the following steps: a parent preparation step: carrying out Suzuki coupling reaction on a tetraphenyl ethylene derivative and pyridine boronic acid to generate a parent unit; and a salt forming step: adopting the parent unit and the connection reactive group unit to generate a target probe capable of detecting PPi and PFOS through a salt forming reaction. The preparation method disclosed by the invention is simple, environment-friendly and good in operability; the probe shows nM-level sensitivity in PFOS (perfluorooctane sulfonate) detection, shows obvious'open 'type fluorescence response in pyrophosphoric acid detection, and has the detection limit as low as nM level.

The present invention relates to the field of medical intermediates, and provides a preparation method for a key intermediate tert-butyl (3aR,5S,6aS)-5-(methylamino)hexahydrocyclopenta[c]pyrrole-2(1H)-carboxylate mesylate of a JAK kinase inhibitor. The method comprises: reacting tert-butyl cis-5-oxohexahydrocyclopenta[C]pyrrole-2(1H)-carboxylate as a raw material with a methylamine equivalent to obtain intermediate A; and then carrying out a reduction reaction in metallic sodium and isopropanol to obtain a crude product, adding L-DBTA to form a salt, removing isomers, and then carrying out re-liberation and salt formation with methanesulfonic acid to obtain a purified product. The method significantly reduces reaction steps, reduces raw material costs, has a simple and reliable process, and is easy for industrial production.

The present invention provides a production method suitable for industrial production of (2S,3S)-3-amino-2-(3-bromo-2-fluorobenzyl)pyrrolidine having a protecting group at the 1-position.The present invention is a method for producing N-[(4-methylphenyl)sulfonyl]-L-phenylalanine salt of (2S,3S)-3-amino-2-(3-bromo-2-fluorobenzyl)pyrrolidine having a protecting group at the 1-position, which comprisesStep 2: a step of subjecting 2-(3-bromo-2-fluorobenzyl)-3-(methoxyimino)pyrrolidine having a protecting group at the 1-position to a reduction reaction; andStep 3: a step of subjecting the product obtained in Step 2 to optical resolution using salt formation with N-[(4-methylphenyl)sulfonyl]-L-phenylalanine.

The present invention provides a method for preparing enantiopure α-methoxyphenylacetic acid. The method comprises: using (R / S)-mandelic acid as the main raw material, performing an O-alkylation reaction with a methylating agent in the presence of an alkaline reagent, followed by purification and dissociation using an organic base to obtain enantiopure α-methoxyphenylacetic acid with a purity of up to 99.0%. The method achieves a maximum yield of 88.6% in an aprotic mixed solvent. This process reduces the amount of methylating agent used and increases the conversion rate to 99.5%. The organic base salt formation purification is efficient, produces a good crystal form, and is easily filtered. The process is simple, highly safe, and suitable for industrial-scale production.

The application relates to the technical field of permanent ferrite preparation, in particular to a method for preparing strontium ferrite by a multi-field coupling auxiliary molten salt method. First, a chemical coprecipitation method is improved to obtain a mixture containing an excess precipitant, inorganic salt and strontium ferrite precursor; then the mixture is subjected to heat treatment under multi-field coupling; finally, strontium ferrite powder is obtained after washing and drying. The application simplifies the chemical coprecipitation process, avoids Sr loss and realizes in-situ salt formation; a multi-element molten salt system is constructed during heat treatment, and an alkali-containing molten salt system with activation is proposed; in the molten salt liquid phase environment, multi-physical fields such as magnetic fields and ultrasonic vibration force fields are cooperated to control the orientation and growth of grains, new driving force and fast channels are provided for ion diffusion, and the rapid synthesis of strontium ferrite and the control of microstructure and size are realized in a low temperature and short time.

This invention relates to the field of materials technology, and more particularly to a 3D-printed, internally hollowed-cone solar interface evaporator with directional salt deposition function, its preparation method, and its application. The invention includes step 1: three-dimensional model construction; step 2: substrate surface pretreatment and chemical activation; and step 3: hydrothermal preparation of a Co-Bi-S coating. This invention uses a 3D-printed porous, internally hollowed-cone resin device as a substrate, and grows a Co-Bi-S coating in situ on its surface using a hydrothermal method. This coating exhibits both excellent photothermal conversion performance and corrosion resistance. The evaporator structure is designed as a porous, internally hollowed-cone shape, which provides a larger evaporation area, stronger light capture and focusing capabilities, and can achieve higher evaporation temperatures and directional salt deposition effects. The prepared solar interface evaporator exhibits excellent photothermal conversion performance and water evaporation efficiency, and also demonstrates good structural stability and corrosion resistance. This solves the technical problems of low photothermal conversion efficiency and poor stability in high-salt environments inherent in traditional solar evaporators, making it suitable for applications such as seawater desalination.