209 results about "Methylpyridinium" patented technology

Provided herein is a process for preparing compound A comprising (a) admixing 2-isopropyl-4-methylpyridin-3-amine (Compound B), or a salt thereof, a first base, and a reactive compound comprising phosgene or a phosgene equivalent in an organic solvent to form 3-isocyanato-2-isopropyl-4-methylpyridine (Compound C); (b) admixing Compound C and 2,6-dichloro-5-fluoronicotinamide (Compound D) to form 2,6-dichloro-5-fluoro-N-((2-isopropyl-4-methylpyridin-3-yl)carbamoyl)nicotinamide (Compound E); and (c) admixing Compound E and a second base to form a product mixture comprising Compound A and the second base. Also provided herein is a process for synthesizing AMG 510 comprising using Compound A prepared according to the disclosed processes

The invention discloses a method for synthesizing 2-vinylpyridine by a one-pot method, which comprises the following step: by taking 2-methylpyridine and paraformaldehyde as raw materials and water as a solvent, synthesizing the 2-vinylpyridine by a one-pot reaction under the catalysis of a basic catalyst. According to the invention, 2-methylpyridine and paraformaldehyde are taken as initial raw materials, the raw materials are simple and easy to obtain, the production cost is reduced, and water is taken as a solvent, so that the use of a large amount of organic solvents is avoided, and the influence on environmental pollution is small. In the reaction, a basic catalyst such as triethylamine is used as a catalyst, a small amount of sodium hydroxide solid is added in the reaction process, the basic catalyst enables the whole system to be in an alkaline environment, and sodium hydroxide improves the depolymerization efficiency of paraformaldehyde and promotes the dehydration process of the reaction, so that the selectivity and yield of 2-vinylpyridine are improved.

Methods are provided for treating or preventing colorectal cancer, related diseases, or symptoms of any of the foregoing, e.g., familial adenomatous polyposis (FAP), in subjects of 55 years or older. The methods include administering 3-[(2R)-2,3-dihydroxypropyl]-6-fluoro-5-(2-fluoro-4-iodoanilino)-8-methylpyrido[2,3-d]pyrimidine-4, 7-dione or a pharmaceutically acceptable salt thereof.

The invention relates to the technical field of organic synthesis, in particular to 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine as well as a synthesis method and application of the 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine. The synthesis method comprises the following steps: (1) synthesizing 2-chloro-3-fluoro-4-iodine-5-methylpyridine from 2-chloro-3-fluoro-5-methylpyridine and an iodine elementary substance to obtain 2-chloro-3-fluoro-4-iodine-5-methylpyridine; (2) synthesizing 2-(2-chloro-3-fluoro-5-methylpyridine-4-yl) benzaldehyde from the 2-chloro-3-fluoro-4-iodo-5-methylpyridine, the 1, 1-bis (diphenylphosphine) ferrocene palladium dichloride, the tripotassium phosphate and the (2-formyl phenyl) boric acid, and further synthesizing the 2-(2-chloro-3-fluoro-5-methylpyridine-4-yl) benzaldehyde from the 2-chloro-3-fluoro-4-iodo-5-methylpyridine and the 1, 1-bis (diphenylphosphine) ferrocene palladium dichloride. And (3) synthesizing the 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine by using the 2-(2-chloro-3-fluoro-5-methylpyridine-4-yl) benzaldehyde and sodium tert-butoxide. The 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine compound constructed by the invention can be used for detecting the content of pesticide residue glyphosate.

The invention relates to the technical field of nicotinic acid synthesis, and particularly discloses an efficient nicotinic acid synthesis method based on step-by-step feeding dynamic control, which comprises the following specific steps: step 1, uniformly dividing potassium permanganate into 3 parts, adding the potassium permanganate into an aqueous solution containing 3-methylpyridine every 15 + / -5 minutes, and supplementing 5-8mL of water after each addition; 2, reacting at 70-90 DEG C for 2-4 hours, and filtering while the solution is hot; 3, adding sodium dithionite into the filtrate, wherein the mass of the sodium dithionite is 0.4-0.6 time that of the potassium permanganate; and 4, concentrating the filtrate to 30-50% of the original volume, adjusting the pH value to 3.0-3.5 with acid, and crystallizing to obtain the nicotinic acid. The method has the following effects: the yield is up to 89.52% at most; the cost is reduced: the consumption of hydrochloric acid is reduced by 77%, and the consumption of potassium permanganate is optimized by 16.7%; the efficiency is improved; the reaction time is shortened by 50%; the large fluctuation of the reaction temperature is controlled through step-by-step feeding, the problem that the reaction liquid which is not completely reacted is too alkaline is solved by filtering and adding sodium dithionite, and the false yield is eliminated through the purification and concentration step while the yield is further improved.

The present invention provides an acid salt of a Sigma-1 receptor agonist or a crystal form thereof, and a preparation method and application thereof. Specifically, it relates to an acid salt of 5-((2-(cyclopropylmethyl)-1,2,3,4-tetrahydroisoquinolin-7-yl)(isopropyl)amino)-1-methylpyridin-2(1H)-one having high affinity for the sigma-1 receptor and a crystal form thereof. The present invention relates to a preparation method of the acid salt and the crystal form and its application in the pharmaceutical field. The acid salt of the compound 5-((2-(cyclopropylmethyl)-1,2,3,4-tetrahydroisoquinolin-7-yl)(isopropyl)amino)-1-methylpyridin-2(1H)-one and the crystal form thereof provided by the present invention have improved physical and chemical properties, such as appearance, hygroscopicity and chemical stability.

The present invention relates to the use of cationic porphyrins such as zinc tetra(N-methylpyridyl)porphyrin tetrachloride and tetra(N-methylpyridyl)porphyrin tetrachloride or a mixture thereof, as selective foliar herbicidal agent.

This invention discloses a method for synthesizing 4-methylpyridine using a Pd / LDH catalyst, belonging to the field of organic chemical synthesis technology. The method includes the following steps: S1, preparing the Pd / LDH catalyst: mixing an aqueous PdCl2 solution with a Mg-Al type LDH support, impregnating at room temperature, drying, and then reducing to obtain the Pd / LDH catalyst; S2, under an inert atmosphere, adding 4-methylpiperidine, the Pd / LDH catalyst, and a low-toxicity solvent to a reaction vessel, stirring the reaction, and then separating and purifying to obtain 4-methylpyridine. This invention, through the combination of a supported Pd / LDH catalyst and a low-toxicity solvent, achieves comprehensive improvements in catalytic efficiency, environmental friendliness, ease of operation, and economy, representing a promising green synthesis route; the reaction conditions are mild, the operation is simple, and the catalyst can be recycled more than 5 times, making it suitable for industrial production.

The invention is applicable to the technical field of non-porous self-adaptive crystals, and provides an application of a non-porous self-adaptive crystal in adsorption and release of 3-methylpyridine, and the non-porous self-adaptive crystal is methyl tetrafluoro column five Me4FP5. The nonporous self-adaptive crystal methyl tetrafluoro column 5 Me4FP5 prepared by the method is applied to the field of 3-MP, controllable release of 3-MP can be realized only by adding an exogenous competitive object, and the released material can also be used for multiple non-thermal stimulation adsorption-release cycles of 3-MP.

The invention discloses a method for preparing 6-fluoronicotinic acid based on a heterogeneous catalytic system, which comprises the following steps: sequentially adding 2-fluoro-5-methylpyridine and a heterogeneous catalyst into a reaction kettle, and uniformly stirring and mixing; continuously introducing oxygen into the reaction kettle, heating to carry out oxidation reaction, monitoring the reaction by HPLC (High Performance Liquid Chromatography) and TCL until the conversion rate of 2-fluoro-5-methylpyridine in a reaction system is greater than or equal to 95%, then cooling to room temperature, filtering reaction liquid, washing a filter cake, drying and recovering the catalyst; after deionized water is added into the filtrate for dilution, a hydrochloric acid solution is added into the reaction system to adjust the pH value, then standing and precipitating are conducted, finally filtering is conducted, and a filter cake is dried to obtain 6-fluoronicotinic acid; the heterogeneous catalyst is a Zr-MOF (Metal Organic Framework) material loaded with TEMPO (Tetramethylpiperidine Oxide)-Cu. According to the method, 2-fluoro-5-methylpyridine is used as a raw material and a reaction medium at the same time, oxygen is used as an oxidizing agent, the 6-fluoronicotinic acid is efficiently synthesized under the catalysis of the heterogeneous catalyst, and the method is low in cost, high in product purity and yield and environmentally friendly.

This application relates to processes and intermediates for the preparation of the PD-1 / PD-L1 inhibitor (R)-1-((7-cyano-2-(3′-((2-(difluoromethyl)-7-((3-hydroxypyrrolidin-1-yl)methyl)pyrido[3,2-d]pyrimidin-4-yl)amino)-2,2′-dimethyl-[1,1′-biphenyl]-3-yl)benzo[d]oxazol-5-yl)methyl)piperidine-4-carboxylic acid, and salts and crystalline forms thereof, where the PD-1 / PD-L1 inhibitor and solid forms and salt forms thereof are useful in the treatment of various diseases including infectious diseases and cancer.

A pharmaceutical composition comprising Compound 1, (3-(6-(1-(2,2-difluorobenzo[d][1,3]dioxol-5-yl) cyclopropanecarboxamido)-3-methylpyridin-2-yl)benzoic acid), and at least one excipient selected from: a filler, a disintegrant, a surfactant, a binder, and a lubricant, the composition being suitable for oral administration to a patient in need thereof to treat a CFTR mediated disease such as Cystic Fibrosis. Processes of preparing pharmaceutical compositions comprising Compound 1 are also disclosed.

The invention discloses a PBT composite material and a preparation method thereof, and relates to the technical field of modified PBT composite materials. The invention provides a polybutylene terephthalate composite material. The polybutylene terephthalate composite material is prepared from the following components in parts by weight: 50-85 parts of polybutylene terephthalate, 1-10 parts of a titanium dioxide coloring agent, 1-10 parts of an acrylic acid toughening agent, 6-20 parts of ionic liquid and 0.1-1.5 parts of an antioxidant, the ionic liquid is composed of positive ions and negative ions, the positive ions comprise at least one of 1-methylpyridinium ions, 1-butylpyridinium ions, 1-butyl-4-methylpyridinium ions, 1-allyl-1-methylpyrrolidinium ions and 1-butyl-1-methylpyrrolidinium ions, and the negative ions comprise at least one of 1-methylpyridinium ions, 1-butylpyridinium ions, 1-butyl-4-methylpyridinium ions, 1-allyl-1-methylpyrrolidinium ions and 1-butyl-1-methylpyrrolidinium ions. The anions comprise at least one of chloride ions, bromide ions, iodide ions and bis (trifluoromethylsulfonyl) imine ions. Through the special compounding effect of all the components, the polybutylene terephthalate composite material with good fluidity and excellent hydrolysis resistance is prepared.

The invention relates to the technical field of anode materials, in particular to a modified carbon anode and a preparation method thereof, and the preparation method comprises the following steps: S1, crushing pretreatment; s2, mixing; s3, extrusion forming; s4, strengthening treatment; the performance of the modified carbon anode in the aspects of conductivity, density, breaking strength and the like can be remarkably improved by matching a unique preparation process with specific components. The double modified asphalt plays a key role in bonding and performance optimization. In the first modification, 2, 3, 5-trimethylpyridine reacts with asphalt, so that the aromaticity and the crosslinking degree of the asphalt are increased, and the softening point and the thermal stability of the asphalt are greatly improved. And the asphalt can stably wrap the asphalt coke particles to form a compact structure, so that the density of the anode is effectively improved. In the second modification, a boron-containing compound is introduced and further reacts with the first modified asphalt to form a boron-containing cross-linked structure, so that not only is the intermolecular force enhanced, but also the crystal structure of the anode is optimized.

The invention relates to the technical field of organic synthesis, and particularly discloses a synthesis method of 4, 4 '-methylene bis (N-cyclohexylcyclohexane-1-amine). The method comprises the following steps: mixing cyclohexanone and 2-methylpyridine borane, and heating to a reaction temperature; the preparation method comprises the following steps: reacting 4, 4 '-diaminodicyclohexylmethane with heat preservation, after the reaction is finished, cooling to room temperature, mixing a reaction solution with diluted hydrochloric acid, adding an organic solvent for extraction, collecting a water phase, then adjusting the pH value of the water phase to 8-9, adding an organic solvent for extraction, collecting an organic phase, drying and concentrating to obtain the 4, 4'-methylene bis (N-cyclohexylcyclohexane-1-amine). The synthesis method provided by the invention has the advantages of simple process, no need of high temperature and high pressure, mild and controllable reaction conditions, no influence of water in a reaction system, high conversion rate and good selectivity, conforms to the concept of green and safe production, and has a good development prospect.

The invention discloses an azide modified platinum radiotherapy sensitizer as well as a preparation method and application thereof. The azide modified platinum radiotherapy sensitizer is an azide modified platinum complex, comprises a cis platinum complex and a trans platinum complex, and is characterized in that the structure of the azide modified platinum radiotherapy sensitizer is shown in the specification; in the formula I, R1 is cyclohexylamine or 2-methylpyridine; in the formula II, R2 is ammonia molecules or pyridine. The azide modified platinum radiotherapy sensitizer can generate a platinum-nitrogen-bin free radical under the irradiation of X rays, and by utilizing a nitrogen transfer reaction in organic chemistry, the platinum-nitrogen-bin free radical generated after the compound is irradiated by rays can be covalently coupled with some DNA (Deoxyribose Nucleic Acid) or protein, so that the sensitivity of the radiotherapy sensitizer is improved. The radiotherapy sensitization effect in tumor radiotherapy is achieved by directly damaging DNA and hindering DNA repair.

The present invention relates to: a tablet comprising 6-((5-methyl-3-(6-methylpyridin-3-yl) isoxazol-4-yl) methoxyl)-N-(tetrahydropyran-4-yl) pyridazine-3-carboxamide; and a pharmaceutical composition comprising the tablet. A process for the preparation of the tablet; a cartridge containing the tablet; and the use of the tablet in medical treatment.

The application relates to the technical field of chemical synthesis, and particularly discloses a production method of 2-amino-5-methylpyridine. The production method obtains 2-amino-5-methylpyridine with high yield and high selectivity through (1) an amination reaction and (2) post-treatment, and has the advantages of short cycle, high equipment utilization, large batch yield, low total production cost, less waste and the like.

The present invention belongs to the technical field of biological catalysis and organic synthesis, and in particular, relates to an imine reductase mutant, application thereof and an application method therefor. The imine reductase mutant has an amino acid sequence derived by a mutation occurring to an amino acid sequence as set forth in SEQ ID NO. 1, and an mutation site includes one of the following sites: position 44 with G mutating into V, or position 89 with L mutating into V, or positions 44 and 89 with G and L simultaneously mutating into V, respectively. The imine reductase mutant of the present invention binds to glucose dehydrogenase to prepare an intermediate (S)-2-methyl-5-(pyrrol-2-yl)pyridine through asymmetric hydrogenation reduction by taking β-nicotinamide adenine dinucleotide disodium salt as a coenzyme and 5-(3,4-dihydro-2H-pyrrol-5-yl)-2-methylpyridine as a substrate, with a chemical conversion rate up to above 99.5% and e.e. % up to 99.6%.

The invention discloses a porphyrin dication covalent metal organic framework material as well as a preparation method and application thereof, and belongs to the technical field of biological medicines. The porphyrin dication covalent metal organic framework material is obtained by copolymerization of porphyrin with methyl, a bipyridine ruthenium (II) complex with aldehyde group and alkyl ammonium bromide. The porphyrin with methyl is tetra (6-methylpyridine-3-yl) porphyrin; the dipyridyl ruthenium (II) complex with the aldehyde group is tris (4, 4 '-dicarboxyaldehyde-2, 2'-dipyridyl) ruthenium (II); the alkyl ammonium bromide is 2-bromoethyl trimethyl ammonium bromide. According to the invention, the CRuP-COF is prepared by utilizing a Knoevenagel condensation reaction and an SN2 nucleophilic substitution reaction through a one-pot method. The CRuP-COF can be used as an intelligent therapeutic agent and can be used as a trinity intelligent treatment platform, photo-thermal / photodynamic / cation cascade collaborative treatment is realized, and healing of open bacterial infected wounds is remarkably accelerated.

The present invention discloses a pinanyl fluorescent probe for detecting the organophosphorus pesticide methyl parathion based on an enzyme inhibition mechanism, as well as its preparation method and application. The fluorescent probe is: 4-(2-(4-(cyclopropylformyloxy-4′-(6,6-dimethyl-2-(4-nitrophenyl)-4,5,6,7-tetrahydro-2H-5,7-methyleneindazole-3-yl)-[1,1′-biphenyl]-3-yl)vinyl)-1-methylpyridinium iodide (abbreviated as: THIP-OCP). The compound can undergo enzymatic hydrolysis reaction with butyrylcholinesterase and, under irradiation with ultraviolet light at a wavelength of 365nm, The solution's fluorescence color changes from colorless to orange-yellow. Since methyl parathion effectively inhibits butyrylcholinesterase activity, when methyl parathion is added to the solution, the solution's fluorescence gradually changes from orange-yellow to colorless under ultraviolet irradiation at a wavelength of 365 nm. Therefore, this compound can be used as a fluorescent probe for detecting methyl parathion. This compound has many advantages, including a low detection limit (0.79 μg / mL) and a wide pH range (5-10), and has great application prospects.

The application discloses a new method for preparing a lumacaftor intermediate. The method uses 5-bromo-6-chloropyridin-2-amine as a starting material, methyl boronic acid, palladium acetate and a ligand L1 to obtain a methylation product. Then, the methylation product is subjected to a Suzuki coupling reaction with m-tert-butoxycarbonyl phenyl boronic acid under the catalysis of tris(dibenzylideneacetone)dipalladium and a ligand L2 to synthesize 3-(6-amino-3-methylpyridin-2-yl)benzoic acid tert-butyl ester. The method can synthesize 3-(6-amino-3-methylpyridin-2-yl)benzoic acid tert-butyl ester at a high yield, and the method uses a small amount of catalyst, has mild reaction conditions and is easy to separate, so that the method is beneficial to industrial implementation and application promotion.

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.

The invention discloses a DASAs molecular optical switch capable of realizing solid film isomerization and a synthesis method and application thereof. The DASAs molecular optical switch is 5-((2Z, 4E)-5-(benzyl ((4-methylpyridine-2-yl) methyl) amino)-2-hydroxypent-2, 4-diene-1-subunit)-2, 2-dimethyl-1, 3-dioxane-4, 6-diketone, 4-methylpyridine-2-formaldehyde reacts with benzylamine, then N-benzyl-1-(4-methylpyridine-2-yl) methylamine is synthesized through reduction of sodium borohydride, and then the DASAs molecular optical switch is obtained. The preparation method comprises the following steps: reacting 2, 3-dimethoxy-1, 3-dioxane-4, 6-diketone in methanol, and reacting with 5-(furan-2-yl methylene)-2, 2-dimethyl-1, 3-dioxane-4, 6-diketone in methanol to synthesize the compound. The DASAs molecular photoswitch disclosed by the invention has rapid and reversible isomerization response to visible light and shows remarkable selective color response to metal ions, and in addition, the molecular photoswitch can realize reversible photochromism in a solid state in a polymer substrate. More importantly, the pure-phase solid film prepared by the molecular optical switch can realize photoisomerization, and has huge application potential in the fields of optical information storage and information permanent encryption, metal ion detectors and the like.

The invention discloses a purification method of 2-cyanopyridine, and belongs to the technical field of chemical engineering. The purification method of the 2-cyanopyridine comprises the following steps: in the process of preparing a 2-cyanopyridine crude product by taking 2-picoline as a raw material through ammonia oxygen catalysis, performing adsorption and impurity removal on the obtained 2-cyanopyridine crude product through an adsorption column filled with a metal adsorbent to obtain the pure 2-cyanopyridine, the metal adsorbent is formed by compounding two or more metals of Li, Cs, Be and Rb with graphene. According to the method, the 2-cyanopyridine with the purity of 99.8% can be purified to 99.99%, the high-quality 2-cyanopyridine is obtained, meanwhile, the reflux ratio does not need to be increased, the rectification energy consumption is reduced, and the cost is reduced; and moreover, the obtained high-quality 2-cyanopyridine is prolonged in preservation time, does not change color, and improves the market share.

The present invention relates to a method for efficiently producing a compound derived from the commercially available and readily available 3-((3S)-7-bromo-2-((2-hydroxypropyl)amino)-5-(pyridin-2-yl)-3H-benzo[e][1,4]diazepine-3-yl)propionate methyl ester, namely, the compound 3-[(4S)-8-bromo-1-methyl-6-(2-pyridinyl)-4H-imidazo[1,2-a][1,4]benzodiazepine-4-yl]propionate methyl ester benzenesulfonate (remimazolam besylate).

The application discloses a preparation method of a catalyst for synthesizing pyridine from 3-methylpyridine and relates to the technical field of catalysts. The catalyst comprises the following steps: ZSM-5 is used as a carrier, V2O5, CoO and Ag are used as active components, molecular sieve ZSM-5, citric acid, ammonium metavanadate, cobalt nitrate, silver nitrate and deionized water are mixed, and then are filtered, dried and calcined to obtain a supported high-efficiency catalyst; the catalyst is filled in a fixed bed, 50% 3-methylpyridine is used as raw material, and a demethylation reaction is carried out under the action of high temperature, the catalyst and air to produce pyridine. The catalyst used in the application does not need to be frequently activated, the activation frequency is low, the catalyst stability is good, the catalyst is not prone to deactivation, can continue to operate stably after activation, catalyst loss is greatly reduced, 3-methylpyridine can be efficiently converted into pyridine by using the prepared catalyst, and the dilemma of waste caused by small demand for 3-methylpyridine in the market is solved.