96 results about "CMN pyrazole" patented technology

The invention discloses a selective etching solution for a titanium and / or copper metal layer of a circuit board and a preparation method of the selective etching solution, and the selective etching solution comprises the following components: 10-20% of persulfate, 4-8% of o-nitrobenzenesulfonate, 0.5-1% of phosphoric acid, 0.2-0.8% of 3-(aminomethyl) pyrazole, 0.3-1.5% of ammonium fluoride, 2-5% of cyclohexanediamine tetraacetic acid, 0.1-0.5% of cyclodextrine and the balance of water. The etching solution can selectively etch a titanium and / or copper metal layer, through selection and cooperation of etching solution components, etching is uniform and stable, taper angle and lateral etching control is good, metal wires are smooth, no metal residues exist, and a good etching solution is provided for the circuit board etching process.

The invention relates to a preparation method of 1-methyl-5-hydroxypyrazole, which comprises the following steps: (a) methylation reaction: fully dissolving pyrazole in a reaction solvent a, dropwise adding a methylation reagent into the reaction solvent a to carry out methylation reaction, adding water into the reaction solvent a to carry out quenching reaction after the reaction is completed, fully washing and concentrating to generate 1-methylpyrazole; (b) bromination hydrolysis reaction: fully dispersing 1-methylpyrazole in a reaction solvent b, dropwise adding bromine into the reaction solvent b to perform bromination reaction, dropwise adding liquid caustic soda and a sodium thiosulfate solution into the reaction solvent b to perform quenching reaction after the reaction is completed, adding the liquid caustic soda into the reaction solvent b after extraction and concentration, and performing heating hydrolysis and cooling crystallization to obtain the 1-methyl-5-hydroxypyrazole. The preparation method of the 1-methyl-5-hydroxypyrazole is reasonable in design, not only reduces the isomer 1-methyl-3-hydroxypyrazole, but also avoids the use of liquid with pungent smell, such as ethylenediamine, and precursor reagents, such as methylhydrazine, improves the operation safety, is environment-friendly, and is beneficial to industrial production.

The present invention relates to a ternary insecticidal composition of 3-[benzoyl(methyl)amino]-N-[2-bromo-4-(1,1,1,2,3,3,3-heptafluoropropan-2-yl)- 6-(trifluoromethyl)phenyl]-2-fluorobenzamide (Component A), 4-chloro-5-ethyl-2-methyl-N-[[4-(4-methylphenoxy)phenyl]methyl] pyrazole-3-carboxamide (Component B) and at least one insecticide (Component C) demonstrating an effective and synergistic broad spectrum control of insects-pests and mites with one shot application by developing delay in resistance of hard to kill and resistant towards insects-pests and mites Further, the ternary insecticidal composition provides residual control and increases yield of treated plants due to protection against insect-pests and mites. The ternary insecticidal composition of present invention increases overall health and plant vigor and is environmentally safe.

Provided are crystalline forms of N-methyl-N-((1s,3s)-3-methyl-3-((6-(1-methyl-1H-pyrazol-4-yl)pyrazolo[1,5-a]pyrazin-4-yl)oxy)cyclobutyl)acrylamide, pharmaceutical compositions, methods of use and methods of making thereof.

The invention provides a nitrification inhibitor for promoting root hair growth, a biostimulant and a preparation method and application of the biostimulant, the nitrification inhibitor comprises 3, 4-dimethylpyrazole and streptomyces fermentation liquor with the weight ratio of 1: (2.5-4.0), and the streptomyces fermentation liquor contains organic acid. The nitrification inhibitor provided by the embodiment of the invention can effectively promote the growth of root hair, further, the biostimulant prepared from the nitrification inhibitor can effectively induce up-regulation expression of auxin related genes ZmARF10, ZmYUC2, ZmYUC3, ZmYUC5, ZmPIN1 and ZmPIN9, the growth of crop root hair is promoted, the root activity of plants is greatly improved, the high-quality growth and yield of crops are promoted, and meanwhile, the biostimulant has good application prospects. The raw materials of the biostimulant are easy to obtain, the preparation method is simple, and industrialization is easy to realize.

The compound cis)-N—((S)-1-(6-(4-fluoro-1H-pyrazol-1-yl)pyridin-3-yl)ethyl)-1-methoxy-4-(4 methyl-6-(5-methyl-1H-pyrazol-3-ylamino)pyrimidin-2-yl)cyclohexanecarboxamide can be prepared as a free base in various crystalline solid forms, and in various salt forms each having one or more solid forms.

The invention belongs to the field of fluorescent sensors, and relates to an Ag-CP fluorescent probe material as well as a preparation method and application thereof. The structural formula of the fluorescent probe material is [Ag (HL) (L)] n, and an HL ligand is 4-(3, 5-dimethyl-1H-pyrazole-1-yl) benzoic acid. Ag-CP is prepared by the following method: dissolving HL and AgNO3 in H2O to obtain light brown turbid liquid, carrying out high-temperature reaction on the light brown turbid liquid, and cooling to obtain the Ag-CP. The Ag-CP material can identify tryptophan (Trp) molecules in an aqueous solution with high selectivity and high sensitivity, has good stability and anti-interference ability in fluorescence identification ability, and can be used as an excellent Trp molecule identification fluorescence sensor.

The present application relates to a kind of preparation method of trifluoromethyl pyrazole compound, belong to the technical field of organic synthesis.The specific method is: (1) trifluoroacetyl ethyl acetate is first with hydrazine hydrate cyclization reaction and generates compound of formula III;(2) under the catalysis of base, compound of formula III is reacted with difluoromethylation reagent and generates compound of formula II;(3) compound of formula II is reacted with methylating agent and obtains compound of formula I;The difluoromethylation reagent is difluoro-monochloromethane or sodium difluoro-monochloroacetate;The methylating agent is chloromethane, bromomethane, iodomethane, dimethyl sulfate or dimethyl carbonate.The present application is prepared by changing reaction route, and the higher-priced raw material methylhydrazine is replaced, and isomer impurity is no longer generated in the product prepared.Not only raw material cost is reduced, but also the purity of product is improved.

The invention relates to the technical field of preparation of pesticide intermediates, and discloses a synthesis method of a pyrazosulfuron intermediate. The preparation method comprises the following steps: (1) in the presence of a palladium catalyst, alkali and an optional ligand, reacting a compound of formula (1) with carbon monoxide and 1, 3-dimethyl-5-hydroxypyrazole to obtain a compound of formula (2); and (2) reacting the compound shown in the formula (2) with sodium methyl mercaptide, and then carrying out oxidation reaction to obtain a compound shown in a formula (3). The intermediate (1, 3-dimethyl-1H-pyrazole-5-(4-trifluoromethyl-2-nitrobenzoyloxy)) provided by the invention is used for further preparing the intermediate 1, 3-dimethyl-1H-pyrazole-5-(4-trifluoromethyl-2-methylsulfonyl benzoyloxy) of the sulfonamide, and the method is simple in process, moderate in reaction condition, simple in post-treatment and high in industrial practicability. # imgabs0 #

The invention discloses a high-temperature-resistant DMPP composite preparation as well as a preparation method and application thereof, and belongs to the technical field of nitrogen fertilizer synergistic materials. The composite preparation is prepared from the following raw materials in parts by weight: 40 to 50 parts of high-molecular compound, 20 to 40 parts of acidic substance, 0.5 to 2.5 parts of lignin sulfonate and 5 to 40 parts of 3, 4-dimethyl pyrazole phosphate DMPP. The compound preparation has good high-temperature resistance and can keep stable chemical properties in the high-temperature granulation process of the fertilizer. In practical application, when the high-temperature-resistant DMPP composite preparation is directly added into fertilizer slurry for high-tower granulation, the stability of DMPP in a high-temperature environment can be ensured, and the decomposition and loss of DMPP caused by high temperature are avoided, so that the effective content of DMPP in a finished product fertilizer is ensured. The problems that the DMPP fertilizer is low in external adding efficiency, the production process is complex, and the cost is additionally increased are solved.

The application belongs to the technical field of organic synthesis and particularly relates to a preparation method of 1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-ol, which comprises the following steps: (1) adding acid into a reaction container, adding 40% methylhydrazine aqueous solution and stirring uniformly; (2) adding trifluoroacetyl acetic acid ethyl ester dropwise into the reaction system of step (1), heating after dropwise addition is completed, performing heat preservation reaction and monitoring the reaction by TLC; (3) after the reaction is completed, adding water into the reaction system of step (2) to perform crystallization, performing suction filtration after cooling, washing the filter cake with water and drying to obtain 1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-ol crude product, and purifying to obtain the final product 1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-ol. The application has the beneficial effect that by controlling the feeding sequence, the acid amount and the reaction temperature, the methylhydrazine addition amount is reduced, methylhydrazine is avoided from being left in waste water, and thus the treatment difficulty of waste water is reduced.

The present invention relates to the field of Mannich base synthesis, and specifically relates to a pyrazole-based ionic liquid 1,2-dibenzyl-3,5-dimethylpyrazolium salt and its synthesis method, and provides a method for catalyzing the Mannich reaction therewith; at room temperature, the pyrazole ionic liquid is used as a catalyst and a solvent, and an aromatic aldehyde, an aromatic amine and cyclohexanone are subjected to a three-component Mannich reaction, and the product and the catalyst are separated with ethanol to obtain the Mannich base β-aminoketone; by screening the types of ionic liquids, solvents, the molar ratios of reactants, the dosage of ionic liquids and reaction temperatures, a series of Mannich bases with higher yields are obtained under the optimized conditions, and the yields are in the range of 77% - 93%. Moreover, the catalyst used is green and effective, has good thermal stability, can catalyze the synthesis of Mannich bases in a short time, the product and the catalyst are easily separated, and the catalyst can be recycled multiple times without obvious reduction in activity.

The present invention belongs to the technical field of organic pigment synthesis, and specifically relates to a preparation method and application of CI Pigment Yellow 183. By using 2-amino-4,5-dichlorobenzenesulfonic acid as a diazo component, using 1-(3'-sulfonate phenyl)-3-methyl-5-pyrazolone (3SPMP) and 1-(3'-sulfonate phenyl)-3-methyl-5-pyrazolone derivatives as coupling components, a long carbon chain alkyl is introduced into the pigment surface, thereby improving the tinting power, fluidity and dispersibility of CI Pigment Yellow 183.

The present application provides methods for preparing (R)-4-(3-((S)-1-(4-amino-3-methyl-1H-pyrazolo[3,4-d]pyrimidin-1-yl)ethyl)-5-chloro-2-ethoxy-6-fluorophenyl)pyrrolidin-2-one, which is useful as a phosphoinositide 3-kinase-delta (PI3Ks) inhibitor, as well as salt forms and intermediates related thereto.

The invention belongs to the field of medicine synthesis, and particularly relates to a preparation method of 3-hydroxy-4-fluorobenzoate. According to the preparation method disclosed by the invention, 3-bromo-4-fluorobenzaldehyde is taken as an initial raw material, and the compound 3-hydroxy-4-fluorobenzoate is prepared through four steps of reactions including aldolization, boronation, oxidation and esterification. The 3-hydroxy-4-fluorobenzoate can be used for preparing the acomidid or an intermediate 3-(3-(3, 5-dimethyl-1H-pyrazol-4-yl) propoxy)-4-fluorobenzoate of the acomidid, and the 3-(3, 5-dimethyl-1H-pyrazol-4-yl) propoxy)-4-fluorobenzoate can be used for preparing the acomidid. The preparation method has the advantages of easily available raw materials, mild reaction conditions, simple operation, high yield and purity, and suitableness for industrial production.

The application discloses a method suitable for reducing N2O emission of straw returned to field in medium-weak acidic soil, and relates to the technical field of environmental protection. The medium-weak acidic soil is the straw full amount smashing and burying returned to field soil, and after pre-culturing the medium-weak acidic soil, nitrogen fertilizer and inhibitor are added into the pre-cultured medium-weak acidic soil in sequence, and after culturing, the N2O emission of the medium-weak acidic soil is reduced. The inhibitor is compounded by 3,4-dimethyl pyrazole phosphate and nano carbon solution. The 3,4-dimethyl pyrazole phosphate and the nano carbon solution have a synergistic effect on reducing the total amount of N2O emission in the medium-weak acidic soil. Specifically, compared with the blank treatment group, the N2O emission amount of the inhibitor prepared by combining the 3,4-dimethyl pyrazole phosphate and the nano carbon solution is reduced by 0.422 kg·hm ‑2 .

A low-density, high-temperature, creep-resistant benzoxazine hybrid epoxy paste and its preparation method are disclosed, relating to the field of adhesive technology. The aim is to address the insufficient long-term high-temperature creep resistance of existing lightweight epoxy adhesives. The paste is prepared from the following raw materials: Raw materials are weighed, and amide-containing trifunctional benzoxazine resin, amide-containing difunctional benzoxazine resin, amide-containing monofunctional benzoxazine resin, multifunctional epoxy resin, bisphenol A type epoxy resin, and toughening agent are added to a reaction vessel. The mixture is heated and stirred to obtain a homogeneous resin premix. The mixture is then cooled, and hollow glass microspheres, a coupling agent, and 2-methyl-pyrazolo[1,5-A]pyrimidine-6-carboxylic acid are added, and the mixture is stirred to obtain an intermediate product. Finally, a curing agent is added and stirred to obtain the low-density, high-temperature, creep-resistant benzoxazine hybrid epoxy paste. This invention is applicable to structural bonding applications in aerospace, rail transportation, and electronic packaging where lightweighting and long-term high-temperature reliability are critical.

A method for preparing a pyrazole derivative 3-bromo-5-methyl-1-H-pyrazole-N-2-chloropyridine (compound of formula I) is disclosed, wherein the method is by reacting a compound of formula II with a halogen-substituted pyridine, or by decarboxylating a pyrazole carboxylic acid of formula XI in the presence of an acid, optionally in the presence of a base and an organic solvent. In addition, a method for preparing a synthetic precursor of formula II, formula IV, formula V, formula VI, formula XI, and a method for preparing a compound of formula VII are provided, including reacting a compound of formula I with an oxidant, optionally in the presence of a catalyst. A compound of formula I as a useful synthetic precursor for preparing an o-aminobenzamide of formula VIII is also disclosed.

The invention belongs to the technical field of energetic materials, and discloses a synthesis method of a fusion casting carrier explosive 4-methoxy-1-methyl-3, 5-dinitropyrazol, commercially available 1-methylpyrazole-4-boronic acid pinacol ester is used as a raw material, a key intermediate 4-methoxy-1-methyl-1H-pyrazole is synthesized through a one-pot method two-step substitution reaction, and the fusion casting carrier explosive 4-methoxy-1-methyl-3, 5-dinitropyrazol is obtained. The product does not need to be purified, and can be directly nitrified after simple post-treatment, so that the casting carrier explosive product 4-methoxy-1-methyl-3, 5-dinitropyrazole is obtained. Compared with the prior art, the preparation method provided by the invention has the advantages of simplicity, high efficiency, low cost and the like, and has the potential of large-scale synthesis.

The invention relates to a method for preparing an isoflaucram intermediate, and provides a novel method for synthesizing 3-(difluoromethyl)-5-fluoro-1-methyl-1H-pyrazole-4-carboxylic acid, which is high in yield and low in cost. The total yield reaches 65% or above.

The present disclosure provides an improved method of treating cancer using N-(5-(difluoromethoxy)-1H-pyrazol-3-yl)-1-((tetrahydro-2H-pyran-4-yl) methyl)-1H-pyrazolo [3, 4-b] pyrazine-6-amine, or a pharmaceutically acceptable salt thereof.

The present invention relates to the design and synthesis of a class of novel chiral phosphine ligand, 1,2-bis(diphenylphosphinoalkylamido)-1,2-disubstituted ethane, and use in asymmetric catalytic reactions, such as asymmetric catalytic synthesis of pyrazoline-5-one with a chiral quaternary carbon center, i.e., highly enantioselective synthesis of 3-methyl-4-benzyl-4-(2-butyl-2,3-butadienyl)pyrazoline-5-one by using 3-methyl-4-benzylpyrazoline-5-one and benzyl (2-butyl-2,3-butadienyl) carbonate with tris(dibenzylideneacetone)dipalladium-chloroform adduct and this novel ligand as catalysts. The ligand designed by this present invention has the following advantages: the structure is novel, the synthesis and enlarge are simple, the enantioselective control effect in the practical reaction is excellent, which has a broad application prospect in chiral catalysis.

The present invention relates to mixtures comprising a solid support comprising a urease inhibitor and another solid support comprising a nitrification inhibitor, such as 3,4-dimethylpyrazole phosphate (DMPP) or 2-(3,4-dimethyl-1H-pyrazol-1-yl)succinic acid (DMPSA), to a method for enhancing the nitrification inhibitory effect or for increasing the health of a plant using mixtures of at least one compound I and at least one compound II; to the use of mixtures comprising compounds I and II for increasing the health of a plant.

Applicants disclose methods, uses, and compositions for treating patients suffering from Cushing Syndrome or Cushing Disease (collectively referred to as' CS ') without causing a significant QT interval extension (e.g., the difference of the QT interval after administration from the baseline QT interval by no more than about 10 milliseconds). The therapeutic amount of the heteroaryl ketone fused aza-naphthane compound may be from about 50 mg / day (mg / day) to up to about 500 mg / day, in embodiments, up to about 800 mg / day. The methods, uses, and compositions can shorten QT intervals, and can be used to treat QT prolongation in patients, including CS patients. The treatment may be a treatment administered orally to a fasting patient or an eating patient. The heteroaryl ketone fused aza-naphthane compounds can be administered with meals. The heteroaryl ketone fused aza-naphthane compound may be reracolan, which is (R)-(1-(4-fluorophenyl)-6-((1-methyl-1H-pyrazol-4-yl) sulfonyl)-4, 4a, 5, 6, 7, 8-hexahydro-1H-pyrazolo [3, 4-g] isoquinolin-4a-yl) (4-(trifluoromethyl) pyridin-2-yl) methanone having the following structure (I) # imgabs 0 #

This provides a crystalline form of PF-07104091 that has desirable properties such as high crystallinity, high purity, low hygroscopicity, favorable solubility or mechanical properties, improved manufacturability or filterability, and / or favorable stability. [Solution] A crystal (Form 3) of (1R,3S)-3-[3-({[3-(methoxymethyl)-1-methyl-1H-pyrazole-5-yl]carbonyl}amino)-1H-pyrazole-5-yl]cyclopentylpropan-2-ylcarbamate (PF-07104091) monohydrate is provided, having a powder X-ray diffraction (PXRD) pattern including peaks at 2θ values ​​measured using CuKα radiation at 8.4, 10.1 and 21.5°2θ±0.2°2θ.

The present application relates to 1, 3-dimethyl-5-pyrazole carboxylic acid esters and related compounds, methods for their preparation and methods of their use as perfume and flavor ingredients in food, cosmetic, pharmaceutical, consumer and other compositions and products.

The present invention provides a novel 5-fluoro-1-[(2-fluorophenyl)methyl]-1H-pyrazolo [3, 4-b]pyridine-3-carboximidamide formate compound of formula (IV) and process for preparation thereof. The present invention further provides for the use of compound of formula (IV) for the preparation of vericiguat compound of formula I. The present invention also relates to process for the preparation of vericiguat Modification form II, vericiguat Modification form III, vericiguat monohydrate and dihydrate.

The utility model belongs to the technical field of 5-hydroxy-1-methyl-3-trifluoromethyl-1H-pyrazole preparation, and particularly relates to a pyrazole compound suction filtration device which comprises a Buchner funnel, a suction filtration box, a liquid collection box and a vacuum assembly, the Buchner funnel is connected to the suction filtration box, the vacuum assembly comprises a first guide pipe and a second guide pipe, and the first guide pipe is connected with the liquid collection box. One end of the first guide pipe is connected with the top of the suction filtration box, and the other end of the first guide pipe is connected with the top of the liquid collection box; a third guide pipe is further arranged at the position, close to the top, of the liquid collecting box and connected with a power device. Compared with the prior art, the device disclosed by the utility model can be used for amplifying production and realizing continuous suction filtration, and meanwhile, the stability of the device in an operation process is improved.

Pesticidal mixtures comprising as active compounds 1) at least one pyrazole compound A of formula I: wherein the variables are as defined in the specification, and 2) at least one further compound B selected from 4-[5-(3,5-dichlorophenyl)-5-(trifluoromethyl)-4H-isoxazol-3-yl]-N-[(4R)-2-ethyl-3-oxo-isoxazolidin-4-yl]-2-methyl-benzamide; 4-[(5S)-5-(3,5-dichloro-4-fluoro-phenyl)-5-(trifluoromethyl)-4H-isoxazol-3-yl]-N-[(4R)-2-ethyl-3-oxo-isoxazolidin-4-yl]-2-methyl-benzamide; N-[4-Chloro-3-[[(phenylmethyl)-amino]-carbonyl]-phenyl]-1-methyl-3-(1,1,2,2,2-pentafluoroethyl)-4-(trifluoromethyl)-1H-pyrazole-5-carboxamide; N-[4-chloro-3-(cyclo-propylcarbamoyl)phenyl]-2-methyl-5-(1,1,2,2,2-pentafluoroethyl)-4-(trifluoromethyl)pyrazole-3-carboxamide; N-[4-chloro-3-[(1-cyanocyclopropyl)carbamoyl]phenyl]-2-methyl-5-(1,1,2,2,2-pentafluoroethyl)-4-(trifluoromethyl)pyrazole-3-carboxamide; 2-chloro-N-(1-cyanocyclopropyl)-5-[1-[2-methyl-5-(1,1,2,2,2-pentafluoroethyl)-4-(trifluoromethyl)pyrazol-3-yl]pyrazol-4-yl]benzamide; 2-(3-ethylsulfonyl-2-pyridyl)-3-methyl-6-(trifluoromethyl)imidazo[4,5-b]pyridine, 2-(3-ethylsulfonyl-2-pyridyl)-5-(trifluoromethylsulfonyl)-1,3-benzoxazole; spiropidion, acynonapyr, and benzpyrimoxan; methods and use of these mixtures for combating invertebrate pests such as insects, arachnids or nematodes in and on plants, and for protecting such plants being infested with pests, especially also for protecting plant propagation material as like seeds.