83 results about "Hydrobromide" patented technology

The invention belongs to the technical field of flame retardants, and particularly relates to a melamine hydrobromide flame retardant and a preparation method thereof. The flame retardant disclosed by the invention has a core-shell structure, the core is hydroxylated melamine hydrobromide subjected to surface modification by a silane coupling agent, and the shell is melamine resin synergistically enhanced by ammonium polyphosphate and oxidized cellulose nanofibrils; through silanization treatment, core-shell interface combination is enhanced, and space-time synergy of gas phase and condensed phase flame retardance is achieved through a composite shell; the obtained flame retardant is high in thermal stability in a polymer matrix, the limit oxygen index of a composite material can be remarkably increased after the flame retardant is added, and the flame retardant has a wide application prospect in the field of flame retardance of high polymer materials through a UL-94 V-0 grade test.

The invention discloses preparation and application of an amido-functionalized polyionic liquid catalyst, vinyl imidazole hydrobromide and N-(4-vinyl) benzyl diethylamine are used as monomers, N, N '-methylene bisacrylamide is used as a cross-linking agent, and the amido-functionalized polyionic liquid catalyst is prepared through a free radical copolymerization method. The imidazole / amido functionalized cross-linked PILs with multiple active sites are prepared by one-step synthesis through a hydrothermal polymerization method. The catalyst has catalytic active sites of amido, imidazolyl and Br, so that the catalyst can efficiently catalyze the cycloaddition reaction of CO2 and epoxide at 80 DEG C and normal pressure in the absence of a solvent and a co-catalyst.

The present application relates to a trace neodymium doped phenethylamine lead bromide monocrystal capable of simultaneously enhancing light yield and shortening decay time and application thereof, which solves the technical problem that the prior art is difficult to simultaneously improve light yield and shorten luminescence decay time. The trace neodymium doped phenethylamine lead bromide monocrystal capable of simultaneously enhancing light yield and shortening decay time is prepared by the following steps: 1) weighing; phenethylamine hydrobromide, lead bromide and neodymium bromide are weighed and placed in a glass bottle; the molar ratio of the phenethylamine hydrobromide, lead bromide and neodymium bromide is 2:1:(0.02-0.05); 2) obtaining a precursor solution; N,N-dimethylformamide is added to the glass bottle, heated and stirred until completely dissolved to obtain a precursor solution; 3) obtaining a crystal; the precursor solution is filtered and placed in a glass beaker for crystallization to obtain a neodymium doped phenethylamine lead bromide monocrystal; through adjustment of the crystal band structure by neodymium, the radiation recombination rate is improved.

The present invention provides a pharmaceutically acceptable salt and crystal form of a KIF18A inhibitor, and a preparation method therefor and a use thereof. The pharmaceutically acceptable salt is selected from one or more of a sodium salt, a potassium salt, a hydrochloride, a p-toluenesulfonate, a maleate, a methanesulfonate, an ethanesulfonate, and a hydrobromide of a compound represented by formula (I). The present invention provides the pharmaceutically acceptable salt of the compound represented by formula (I) and a crystal of the salt, which exhibit excellent hygroscopicity, solubility, and / or stability, and are suitable for pharmaceutical use.

The invention provides various salt forms of deuterated dextromethorphan as shown in a formula (I) as well as a preparation method and application of the various salt forms. The various salt forms comprise tartrate, citrate, hydrobromide and benzoate. Also provided are various crystal forms of the above salts. The salt has excellent effects in the aspects of stability, biological activity, bioavailability, drug effect and the like, and is suitable for development of pharmaceutical preparations.

The present invention provides a salt of a triazine compound which has an inhibitory action against aldosterone synthase and is useful as a drug, and especially as a drug for preventing or treating primary aldosteronism and the like, a crystal thereof, and a method for producing the same. Specifically, the present invention provides a pharmaceutically acceptable salt of 3-[4-[[trans-4-(acetamino)cyclohexyl]carbamoylmethyl]piperazin-1-yl]-5-(p-tolyl)-1,2,4-triazine, wherein the salt is hydrobromide, sulfate, succinate, or tosylate, and the like.

The application provides a preparation method of low-impurity vonerogefumate. The application provides a method for removing impurities A-E in the preparation of vonerogefumate, wherein vonerogefumate is reacted with hydrobromic acid to obtain vonerogefumate hydrobromide, and the method specifically comprises the following steps: (1) dissolving vonerogefumate and hydrobromic acid in a solvent; (2) cooling or directly precipitating a solid; and (3) separating to obtain vonerogefumate hydrobromide. The method can remove impurities A-E which are difficult to remove by a recrystallization refining method, and the method has good selectivity for impurities A-E. The application provides an impurity D, a preparation method thereof and application of the impurity D as an impurity control sample of vonerogefumate.

The invention provides a composition containing picocetinib hydrobromide and a preparation method thereof, the composition is a tablet, the active component picocetinib hydrobromide and a hydrophilic gel framework material (e.g., hydroxypropyl methylcellulose, polyoxyethylene resin or hydroxypropyl methyl cellulose acetate succinate) form a solid dispersion, and the solid dispersion is prepared into the composition containing the picocetinib hydrobromide and the hydrophilic gel framework material (e.g., hydroxypropyl methylcellulose, polyoxyethylene resin or hydroxypropyl methyl cellulose acetate succinate). The solubility of the medicine is improved, and stable release in vivo is realized; according to the present invention, with the addition of the pH value adjusting agent, the solubility of the picetinib hydrobromide can be maintained without limitation in the neutral pH region, the stability is good, and the stable release in the body is achieved so as to achieve the rheumatic arthritis treatment effect, improve the patient comfort and the treatment compliance, reduce the administration frequency and the medical cost, reduce the side effect, and provide the clinical application prospect. The whole preparation method is simple and suitable for industrial production.

The invention discloses an analysis method for determining halogenated alkane impurities in tigliptin hydrobromide, and relates to the technical field of quality analysis. In order to solve the problem of detection of halogenated alkane impurities in tigliptin hydrobromide, the invention provides a convenient, efficient and accurate detection method. The method comprises the following steps: preparing a test solution and an impurity reference solution, and detecting by adopting a gas chromatographic method; the method can be used for accurately determining the content of halogenated alkane in tigliptin hydrobromide, plays a guiding role in development of a synthesis process, and contributes to establishment of quality standards of tigliptin hydrobromide bulk drugs.

Provided herein is N-((4,6-dimethyl-2-oxo-1,2-dihydropyridin-3-yl)methyl)-5-(ethyl (tetrahydro-2H-pyran-4-yl)amino)-4-methyl-4′-(morpholinomethyl)-[1,1′-biphenyl]-3-carboxamide hydrobromide. Also provided herein is a particular polymorph form of this compound.

The invention provides an X-ray luminescent crystal material containing heavy atoms as well as a preparation method and application thereof, and belongs to the technical field of luminescent materials. The chemical formula of the X-ray luminescent crystal material is 2XL at-AMnBr4, 2XL represents dihalogen substituted p-phenylenediamine hydrobromide, halogen atoms are one or two of Cl, Br and I, and A represents crown ether. According to the invention, heavy atoms are introduced into the organic cation module of the organic-inorganic hybrid metal halide through the multistage supramolecular self-assembly effect for the first time, the luminescence property and stability of the X-ray luminescent material are improved, and the luminescent quantum yield reaches 60% or more. The X-ray luminescent material provided by the invention is used as a scintillator of a core component, can efficiently convert X-rays into visible light signals, and provides more accurate and rapid analysis and detection for multiple fields such as safety inspection, scientific research, medical diagnosis and the like.

The invention provides a crystal form of a compound HIF-117 salt as well as a preparation method and application of the crystal form, and the crystal form is any one or more of the following crystal forms: a hydrochloride crystal form A, a sulfate crystal form B, a 1, 2-ethanedisulfonate crystal form C1, 1, 2-ethanedisulfonate crystal form C2, 1, 2-ethanedisulfonate crystal form C3 and 1, 2-ethanedisulfonate crystal form C4. The crystal form 1, 2-ethanedisulfonate crystal form C2, p-toluenesulfonate crystal form D, mesylate crystal form E1, mesylate crystal form E2, hydrobromide crystal form F1, hydrobromide crystal form F2, sodium salt crystal form G, sylvite crystal form H1, sylvite crystal form H2, calcium salt crystal form I, magnesium salt crystal form J, choline salt crystal form K, lysine salt crystal form L, ammonium salt crystal form M, meglumine salt crystal form N, betaine salt crystal form O1, betaine salt crystal form O2 and diethylamine salt crystal form P1, the invention relates to a diethylamine salt crystal form P1, a diethylamine salt crystal form P2, a diethylamine salt crystal form P3, a diethylamine salt crystal form P4, a diethylamine salt crystal form P5, a tromethamine salt crystal form Q1, a tromethamine salt crystal form Q2 and a tromethamine salt crystal form Q3. The compound has good stability, and has important value for development and production of medicines and preparations.

The invention relates to a polymorphic form of hydrobromide or hydrochloride of 5-(6-(4-(cyclopropylmethyl) piperazine-1-yl)-2-methylpyridine-3-yl)-N-((4, 6-dimethyl-2-oxo-1, 2-dihydropyridine-3-yl) methyl)-3-(N-ethylcyclopropanecarboxamide)-2-methylbenzamide, a pharmaceutical composition of the polymorphic form and application of the polymorphic form and the pharmaceutical composition of the hydrobromide or hydrochloride of the 5-(6-(4-(cyclopropylmethyl) piperazine-1-yl)-2-methylpyridine-3-yl)-N-(4, 6-dimethyl-2-oxo-1, 2-dihydropyridine-3-yl)-3-(N-ethylcyclopropanecarboxamide.

This application discloses an analytical method for N-nitrosamine vortioxetine in vortioxetine hydrobromide tablets, belonging to the field of pharmaceutical impurity analysis. The method employs high-performance liquid chromatography (HPLC), with the following chromatographic conditions: a 4.6 mm × 250 mm column packed with octadecylsilane-bonded silica gel, with a particle size of 5 μm; mobile phase A is a 90:10 water-acetonitrile mixture containing 0.025%–0.035% trifluoroacetic acid (v / v); mobile phase B is acetonitrile; gradient elution; column temperature 38–42 °C; flow rate 0.9–1.1 ml / min; injection volume 50 μl; and detection wavelength 226 nm. This analytical method effectively eliminates excipient interference and exhibits excellent detection performance (specificity, sensitivity, linearity, precision, accuracy, and robustness), accurately detecting the content of N-nitrosamine vortioxetine in vortioxetine hydrobromide tablets, meeting quality control requirements.

The invention discloses a preparation method of hydrobromic acid vortioxetine, and belongs to the technical field of organic synthesis. The method comprises the following steps: by taking o-aminothiophenol and Boc2O as initial raw materials, carrying out amino protection to obtain an intermediate 1; reacting the intermediate 1 with 2, 4-dimethyl bromobenzene under an alkaline condition to form a thioether bond, and acidifying to obtain an intermediate 2; carrying out high-temperature cyclization on the intermediate 2 and bis (2-bromoethyl) amine hydrobromide in mesitylene, so as to obtain a crude product of the hydrobromic acid vortioxetine; and recrystallizing the crude product with 95% ethanol to obtain a high-purity final product. The route is simple, only three-step reaction is needed, a noble metal catalyst is not needed in the whole process, and the problem of metal residues is fundamentally avoided; the selected raw materials are easy to obtain, the reaction condition is mild, the operation is simple and convenient, the process is stable, the total yield is good, the product purity is as high as 99.9%, and the method is suitable for large-scale production.

The present invention relates to polymorphs of the hydrobromide salt of 5-{2-[({8-[(2,6-dimethylbenzyl)amino]-2,3-dimethylimidazo[1,2-a]pyridin-6-yl}carbonyl)-amino]ethoxy}-5-oxopentanoic acid (linaprazangrate), more specifically Form A, Form B, and Form C of the HBr salt of linaprazangrate. The present invention also relates to pharmaceutical compositions containing such polymorphs and to the use of these polymorphs in the treatment or prevention of gastrointestinal inflammatory or gastric acid-related diseases, particularly erosive gastroesophageal reflux disease (eGERD).

The present invention relates to polymorphs of the hydrobromate of 5-{2-[({8-[(2, 6-dimethylbenzyl) amino]-2, 3-dimethylimidazo [1, 2-a] pyridin-6-yl} carbonyl)-amino] ethoxy}-5-oxovaleric acid (linaraben glutarate), and more particularly to Form A, Form B and Form C of the HBr salt of linaraben glutarate. The present invention also relates to pharmaceutical compositions comprising the polymorphs, and to the use of these polymorphs in the treatment or prevention of gastroenteritis diseases or gastric acid related diseases, in particular erosive gastroesophageal reflux disease (eGERD).

The invention relates to guanidine-containing hydrobromide electrolyte for a high-energy-density zinc-bromine-iodine battery as well as a preparation method and application of the guanidine-containing hydrobromide electrolyte, and belongs to the technical field of aqueous zinc-bromine-iodine batteries. The guanidine hydrobromide-containing electrolyte for the high-energy-density zinc-bromine-iodine battery comprises guanidine hydrobromide, zinc salt and deionized water. According to the guanidine-containing hydrobromide electrolyte for the high-energy-density zinc-bromine-iodine battery, provided by the invention, redox of iodine valence state I-I0I < + > and redox of bromine valence state BrBr0 can be realized at the same time, and six-electron transfer of halogen compounds in the zinc-bromine-iodine battery is realized. On one hand, the energy density of the battery is increased to 3-4 times of the initial value, and on the other hand, the zinc-bromine-iodine battery containing the zinc-bromine-iodine battery has the advantages of being easy to manufacture and easy to industrially popularize.

The present invention provides a pharmaceutically acceptable salt and crystal form of a KIF18A inhibitor, and a preparation method therefor and a use thereof. The pharmaceutically acceptable salt is selected from one or more of a sodium salt, a potassium salt, a hydrochloride, a p-toluenesulfonate, a maleate, a methanesulfonate, an ethanesulfonate, and a hydrobromide of a compound represented by formula (I). The present invention provides the pharmaceutically acceptable salt of the compound represented by formula (I) and a crystal of the salt, which exhibit excellent hygroscopicity, solubility, and / or stability, and are suitable for pharmaceutical use.

The present invention relates to a process for the industrial-scale production of 5-{2-[benzyl-(1-(4-hydroxyphenyl)-1-methylethyl)amino]-1-hydroxyethyl}benzene-1,3-diol hemifumarate, a salt consisting of two molecules of 5-{2-[benzyl-(1-(4-hydroxyphenyl)-1-methylethyl)amino]-1-hydroxyethyl}benzene-1,3-diol and one molecule of fumaric acid, and having the following formula: 5-{2-[benzyl-(1-(4-hydroxyphenyl)-1-methylethyl)amino]-1-hydroxyethyl}benzene-1,3-diol hemifumarate is a useful intermediate in the synthesis of 5-[(1RS)-2-[(1RS)-2-(4-hydroxyphenyl)-1-methylethyl]-amino-1-hydroxyethyl]benzene-1,3-diol hydrobromide, which is used in the pharmaceutical field under the is known by the common name fenoterol hydrobromide.

Novel crystalline forms of Nirogacestat dihydrobromide and preparation methods thereof, pharmaceutical compositions containing the crystalline forms, and uses of the crystalline forms for preparing γ-secretase inhibitor drugs and drugs for treating desmoid tumors.

The preparation method comprises the following specific steps: firstly, taking copper bromide and 1-butyl-3-methylimidazole hydrobromide as raw materials, and reacting to prepare a copper complex ionic liquid; ultrasonically dispersing cerium nitrate and lanthanum-doped lithium titanate into the copper complexing ionic liquid to obtain ionic liquid mixed liquid; stirring and heating tetraethoxysilane to 130-150 DEG C, continuously adding the ionic liquid mixed solution, uniformly stirring and mixing, immediately adding tetrabutyl titanate, concentrated hydrochloric acid, deionized water and methanol, carrying out heat-preservation stirring for 30-40 minutes under the condition of a pulsed magnetic field, finally, carrying out heat-preservation standing for 8-10 hours, and carrying out post-treatment, so as to obtain the ionic liquid. The composite denitration agent disclosed by the invention can be used for flue gas treatment of the lime rotary kiln, can realize a relatively good denitration effect under the condition of low temperature (100-120 DEG C), and has a good popularization prospect.

The present invention relates to a kind of synthesis process of thiabendazole, including:Using lactic acid and o-phenylenediamine as raw materials, solid acid is used as catalyst condensation reaction in water to obtain 2 α hydroxyethyl benzimidazole;2 α hydroxyethyl benzimidazole, micron-grade magnetic iron powder are mixed and put into water, hydrogen peroxide is added for catalytic oxidation, and 2 acetyl benzimidazole is obtained;2 acetyl benzimidazole is put into glacial acetic acid, bromine is added, and the MOF powder of trivalent Fe as central metal is catalyst, bromine substitution reaction is carried out, and 2 dibromoacetyl benzimidazole hydrobromide is obtained;Formamide and phosphorus pentasulfide are put into ethyl acetate, 30 45 DEG C of reaction 1 2h, 2 dibromoacetyl benzimidazole hydrobromide is added, ammonia catalytic cyclization reaction is passed through, and reaction is filtered after terminating, and filtrate cools down and precipitates solid, separates solid, washes, and obtains thiabendazole. The present invention can obtain higher yield than prior art, and reaction conditions are mild, catalyst and solvent are easily separated and recycled, reduces waste of raw materials, and reduces resource recovery difficulty.

Provided are a salt and / or a crystal form of a compound degrading BTK and preparation and application thereof. The pharmaceutically acceptable salt and crystal form of the compound as shown in formula (I), wherein the pharmaceutically acceptable salt is selected from a maleate salt, a fumarate salt, a hydrogen halide salt (preferably a hydrobromide salt and a hydrochloride salt), a sulfate salt, a phosphate salt, an L-tartrate salt, a citrate salt, an L-malate salt, a hippurate salt, a D-glucuronate salt, a glycolate salt, a mucate salt, a succinate salt, a lactate salt, an orotate salt, a pamoate salt, a glycine salt, an alanine salt, an arginine salt, a cinnamate salt, a benzoate salt, a benzene sulfonate salt, a p-toluene sulfonate salt, an acetate salt, a propionate salt, a valerate salt, a triphenylacetic acid salt, an L-proline salt, a ferulic acid salt, a 2-hydroxyethanesulfonate salt, a mandelate salt, a nitrate salt, a methanesulfonate salt, a malonate salt, a gentisate salt, a salicylate salt, an oxalate salt or a glutarate salt:

The present invention relates to the field of thiabendazole preparation, specifically an improved thiabendazole preparation method. Comprise the following steps: S1 methylglyoxal is added to a container, the temperature is raised to 30-35 DEG C to melt, a catalyst is added, stirred evenly, air is blown in, and then o-phenylenediamine and acetic acid are added in batches, and the temperature is raised to 50-60 DEG C after adding, and the reaction is carried out for 2-5h to obtain a reaction solution containing 2-acetylbenzimidazole; S2 The reaction solution obtained in step S1 is added with liquid bromine, reacted, and after the reaction is completed, cooled, filtered, washed, and dried to obtain 2-dibromoacetylbenzimidazole hydrobromide; S3 The 2-dibromoacetylbenzimidazole hydrobromide obtained in step S2 is added to ethyl acetate, and then formamide and phosphorus pentasulfide are added for ring-closure reaction to obtain a closed-loop reaction liquid; S4 The thiabendazole in the closed-loop reaction liquid obtained in step 3 is purified to obtain a thiabendazole product. The process is simple, the prepared product has high purity, and the purity is 99.3%, and it is expected to be industrialized as soon as possible.

The invention provides a passivation solution, a passivation method and a passivation layer for passivating the surface of a perovskite thin film. The passivation solution for passivating the surface of the perovskite thin film contains a metal organic framework material, hydrobromide of a diamine compound and a solvent, the particle size of the metal organic framework material is 30-50nm. The perovskite thin film is passivated by using the mixed solution of the hydrobromide containing the metal organic framework material and the diamine compound, so that surface and carrier recombination can be reduced and inhibited, the electron extraction capability is improved, and the open-circuit voltage and the fill factor are simultaneously improved.

The application relates to a large-size rare earth doped phenethylamine lead bromide perovskite monocrystal preparation method and perovskite monocrystal, and solves the technical problems that the preparation of the existing large-size rare earth doped two-dimensional perovskite monocrystal needs higher nucleation supersaturation, the preparation period is long, and part of the rare earth bromide is extremely easy to absorb moisture, thereby reducing the crystal quality. The large-size rare earth doped phenethylamine lead bromide perovskite monocrystal preparation method and perovskite monocrystal comprise the following steps: 1) weighing; phenethylamine hydrobromide, lead bromide and rare earth metal bromide are weighed and placed in a glass bottle; 2) obtaining a precursor solution; 3) obtaining a millimeter-level size crystal; 4) screening a seed crystal; and 5) seed crystal growth. In step 4), the open container B is placed at a preset temperature until the seed crystal continues to grow into a rare earth doped phenethylamine lead bromide perovskite monocrystal with a predetermined size, and the size can reach a centimeter level, which has an important supporting role in promoting the performance research of the rare earth doped two-dimensional perovskite monocrystal.

The present invention relates to an improved process for preparation of Zastaprazan or its pharmaceutically acceptable salts, which comprises: a) reaction of methyl 5,6- diaminonicotinate and 3-bromobutan-2-one to obtain methyl 8-amino-2,3-dimethyl imidazo[1,2-a]pyridine-6-carboxylate hydrobromide salt, b) reaction of obtained compound in step a) with 2,6-dimethylbenzyl chloride in presence of base in solvent, in absence of catalyst to obtain methyl 8-((2,6-dimethylbenzyl)amino)-2,3-dimethylimidazo[1,2-a]pyridine-6-carboxylate, c) hydrolysis of the obtained compound in step b) in presence of base in a solvent to obtain 8-((2,6-dimethylbenzyl)amino)-2,3-dimethylimidazo[1,2-a]pyridine-6-carboxylic acid d) condensation of obtained compound in step c) with azetidine or its salts in presence of condensing agent, base and solvent to obtain Zastaprazan, wherein condensing agent is selected from PyBOP or T3P.

The present invention provides a salt of a triazine compound which has an inhibitory action against aldosterone synthase and is useful as a drug, and especially as a drug for preventing or treating primary aldosteronism and the like, a crystal thereof, and a method for producing the same. Specifically, the present invention provides a pharmaceutically acceptable salt of 3-[4-[[trans-4-(acetamino)cyclohexyl]carbamoylmethyl]piperazin-1-yl]-5-(p-tolyl)-1,2,4-triazine, wherein the salt is hydrobromide, sulfate, succinate, or tosylate, and the like.

The present application relates to a salt of a triazine compound, a crystal form thereof, and a method for producing the same. Provided are: a salt and a crystal of a triazine compound, which have an inhibitory effect on aldosterone synthetase and are useful as a drug, particularly a prophylactic or therapeutic drug for primary aldosterone hyperplasia and the like; and a method for producing the salt and the crystal of the triazine compound. Specifically, the present invention provides a pharmaceutically acceptable salt of 3-[4-[[trans-4-(acetamido) cyclohexyl] carbamoylmethyl] piperazin-1-yl]-5-(p-tolyl)-1, 2, 4-triazine (wherein the salt is a hydrobromide salt, a sulfate salt, a succinate salt, a p-toluenesulfonate salt, or the like), and a pharmaceutically acceptable salt of 3-[4-[[trans-4-(acetamido) cyclohexyl] carbamoylmethyl] piperazin-1-yl]-5-(p-tolyl)-1, 2, 4-triazine.