134 results about "Dichlofopmethyl" patented technology

The present invention relates to compositions for use in refrigeration and air-conditioning systems comprising 1-ethoxy-1,1,2,2,3,3,4,4,4-nonafluorobutane and at least one chlorocarbon, alcohol, ketone, ether, ester, N-(difluoromethyl)-N,N-dimethylamine, or mixtures thereof. Further, the present invention relates to compositions for use in refrigeration and air-conditioning systems employing a centrifugal compressor comprising 1-ethoxy-1,1,2,2,3,3,4,4,4-nonafluorobutane and at least one chlorocarbon, alcohol, ketone, ether, ester, N-(difluoromethyl)-N,N-dimethylamine, or mixtures thereof. The compositions of the present invention may be azeotropic or near-azeotropic and are useful in processes for producing cooling or heat or as heat transfer fluids.

Fluoroalkyl-substituted, nitrogen-containing, aryl heterocyclic compounds are provided. The compounds are derivatives of pyridine, pyrimidine, or pyrazine, and have two or three functional groups bonded to the heterocyclic ring, including a perfluoroethyl, perfluoropropyl, perfluoroisopropyl, perfluorobutyl, or difluoromethyl group. Methods of making the compounds using a copper reagent are also provided.

The invention relates to a 2-arylsulfonyl-2, 2-difluorodiazoethane compound, a preparation method and application thereof. The preparation method of the 2-arylsulfonyl-2, 2-difluorodiazoethane compound includes: dissolving 2, 2-difluoro-2-aryl sulfonyl ethylamine hydrochloride in a mixed solvent of an organic solvent and water, adding nitrite, carrying out stirring at room temperature for completereaction, and then conducting washing, extraction, separation and column chromatography purification to obtain the yellow liquid 2-arylsulfonyl-2, 2-difluorodiazoethane. The obtained target compoundis a diazo compound containing sulfonyl difluoromethyl, can be subjected to [3+2] cycloaddition reaction with alkyne so as to synthesize a pyrazole compound containing difluoromethyl. The difluorodiazoethane compound provided by the invention has the characteristics of convenient preparation, simple use and mild reaction conditions, and the invention provides an effective method for synthesis of compounds containing difluoromethyl.

The invention discloses a synthesis method of 3-difluoromethyl-1-methylpyrazole-4-formic acid, and belongs to the technical field of difluoromethyl pyrazole synthesis. According to the synthesis method, 3-difluoromethyl-1-methylpyrazole-4-formic acid is prepared from 1-dimethylamino-1-butylene-3-one, difluoroacetyl fluoride, and methyl hydrazine through a series of reactions. The provided synthesis method has the advantages of easily available raw materials and high yield, can be applied to industry, and has a comprehensive yield more than 65%.

The invention discloses a difluoromethyl silver compound, a single crystal, a synthetic method and an application. The invention provides a difluoromethyl silver compound (1a) or a difluoromethyl silver compound (1b), wherein R and R' are independently a phenyl group or a naphthyl group having substituent groups at any position of the phenyl group or the naphthyl group. The substituent group is one or more in number and is an alkyl group with the carbon number of 1-6, an alkoxy group with carbon number of 1-6 or an alkyl-substituted amino group with the carbon number of 1-6, wherein the substituent groups on the phenyl group or the naphthyl group are same or different and the R and R' are same or different. The invention also provides the synthetic method of the difluoromethyl silver compound (1a) or the difluoromethyl silver compound (1b), which includes following steps: carrying out a reaction with aza-carbene complexed silver chloride and trimethyl silyl difluoromethane. The difluoromethyl silver compound is good in stability, can be subjected to an electrophilic substrate through a difluromethylated reaction, is mild in reaction condition, is good in group compatibility and is excellent in market development prospect.

The invention discloses a synthesis method of 2-(difluoromethyl)pyridine-3-ol, and belongs to the field of organic chemical synthesis. The method comprises the following steps: dissolving 3-methoxypyridine-2-formaldehyde into an organic solvent, and performing reaction with diethylamino sulfur trifluoride under the protection of nitrogen to obtain 2-(difluoromethyl)-3-methoxypyridine; and reactingthe 2-(difluoromethyl)-3-methoxypyridine with an acid to obtain the target product 2-(difluoromethyl)pyridine-3-ol. The method is reasonable in process design, short in route, simple in synthesis operation and easy to implement.

The invention discloses a preparation method of 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid ethyl ester, and belongs to the technical field of organic synthesis. The preparation method comprises the following steps: with 1,3-dimethylpyrazole as a raw material, carrying out halogenation to obtain 4-halogenated-1,3,5-tetrahydronaphthalene; carrying out a reaction under the conditions of a bromination reagent and AIBN and hydrolysis with hexamethylenetetramine to obtain 4-halogen-1-methyl-1H-pyrazole-3-formaldehyde, then performing a reaction with a fluorination reagent to obtain 4-halogen-3-difluoromethyl-1-methylpyrazole; finally carrying out a reaction on the 4-halogen-3-difluoromethyl-1-methylpyrazole and a Grignard reagent to obtain 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid ethyl ester. The method is simple and convenient to operate and high in reaction yield, the purity of the obtained product can reach 99.5% or above, and the method has a potential process amplification prospect.

The invention discloses difluromethylphosphonium salt, and a preparation method and application thereof. A synthetic method of the difluromethylphosphonium salt disclosed by the invention comprises the following steps of in a solvent, carrying out a reaction shown as follows on gem-difluoromethylenated phosphonium inner salt as shown in a formula II and protonic acid, and preparing a compound as shown in a formula I. The invention discloses application of the compound as shown in the formula I in difluromethylation reaction with a compound as shown in a formula III or a compound as shown in a formula IV. The preparation method of the difluromethylphosphonium salt provided by the invention is simple and convenient to operate and wide in substrate applicability, can be carried out with the existence of water and oxygen, and is moderate in reaction condition and high in yield and purity. The difluromethylphosphonium salt provided by the invention can be used for directly difluromethylating aldehyde, ketone and imine compounds, and the method is simple to operate, moderate in condition, and high in reaction yield when a substrate is a ketone compound containing alpha-H.

The invention discloses a difluoromethylation Preparation method for 2-(2,4-dichlorophenyl)-1,2-dihydrogen-5-methyl-3H-1,2,4-triazole-3-ketone. The method comprises the following steps: triadimefon is led to react with potassium carbonate to obtain potassium triadimefon using xylol as reaction solvent and in the presence of phase transfer catalyst; the potassium triadimefon is then let to react with chlorodifluoromethane at the temperature of 150-200 DEG C; and the 2-(2,4-dichlorophenyl)-1,2-dihydrogen-5-methyl-3H-1,2,4-triazole-3-ketone is prepared at a high yield. The method is simple and highly efficient, is safe in operation and high in yield, and facilitates industrial production.

The invention discloses a synthesis method for an anti-tumor new medicine 3-{(3-chlorphenyl)difluoromethyl-1-isopropyl-monohydro-pyrazolo(3,4-D)pyrimidine-4-amine compound. The synthesis method comprises the following steps of: acylating 3-chlorphenyl-2 oxalic acid serving as an initiative raw material; reacting the acylated material with dipropionitrile; performing methylation; performing ring closure with hydrazine hydrate to obtain 5-amino-1-(3-chlorophenyl)-pyrazole-4-carbonitrile, crystallizing and purifying, heating and performing ring closure with formamide to obtain a target mother ring; performing fluorination on carbonyl by using DAST; introducing difluorine into an active group so as to improve the bioactivity of the compound; performing process optimization on the basis of the compound; and performing the similar steps by using 2-(3-chlorphenyl)-2,2-difluoroacetic acid as a raw material to obtain the target product.

The invention discloses a synthesis method of a 1, 1-difluoro-2-isonitrile-ethyl phenyl sulfone compound. The synthesis method is characterized in that the 1, 1-difluoro-2-isonitrile-ethyl phenyl sulfone compound is synthesized from a 2, 2-difluoro-2-(thiophenyl) ethyl acetate compound through the steps of reduction, oxidation, alcohol amination, formylation, dehydration reaction and the like. According to the method, reducing agent lithium aluminum hydride which is dangerous and poor in selectivity is prevented from being used for reducing a difluoromethyl amide intermediate low in reaction activity; the mild reducing agent sodium borohydride is adopted to reduce the 2, 2-difluoro-2-( thiophenyl) ethyl acetate compound high in activity, so that the reduction yield and selectivity are greatly improved, and the method is simple to operate, stable in product property and beneficial to large-scale production.

A high yielding extraction process for the purification of N-(2,4-dichloro-5-(4-(difluoromethyl)-3-methyl-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl)methanesulfonamide (sulfentrazone) by selectively partitioning the desired product from the crude mixture, thereby increasing its purity by decreasing the presence of unwanted impurities and improving the color and particle size distribution of the final sulfentrazone product. The selective partitioning is achieved by the sequential use of an organic solvent, water, aqueous inorganic base and a concentrated aqueous inorganic acid.

The invention provides a method for purifying 2-(2-flourine-4-chlorine-5-aminophenyl)-4-difluromethylation-5-methyl-1,2,4-triazole-3-ketone. The method comprises the following steps: firstly, forming an acid from a crude product; decolorizing; and neutralizing to obtain a pure product. The purification process is free of demands on the purity of the crude product; other purifying auxiliary materials are cheap and available; the purifying steps are simple to operate; and industrial production is easy to achieve.

The invention discloses a preparation method of 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, and belongs to the technical field of organic synthesis. The preparation method comprises thefollowing steps: reacting N-methyl-3-aminopyrazole as a raw material with bromine/iodine to replace pyrazole at site 4, then carrying out diazotizing and coupling with potassium difluoromethyl trifluoroborate to obtain 4-bromo-3-(difluoromethyl)-1-methyl-1H-pyrazole, then performing Grignard exchange by adopting isopropyl magnesium chloride and the like, and performing reaction with carbon dioxide to obtain 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid. The method is simple and convenient to operate, the total yield of the three steps is as high as 64%, the product purity can reach 99.5% or above, the situation in which isomers exist in a traditional process is avoided, and the method has potential process amplification prospects.

The invention discloses a method of asymmetric alpha-difluoromethylation of beta-ketoester through phase-transfer catalysis. The method includes: performing stirring reaction on beta-ketoester compound IIIa, a phase-transfer catalyst, TMSCF2Br and alkaline in a solvent at -78 to 60 DEG C with thin-layer chromatography for tracing the reaction until the reaction is finished, layering a mixed liquid; collecting the organic layer and spin-drying the solvent, and performing column chromatography separation to obtain chiral alpha-difluoromethyl-beta-ketoester compound IIIb. The effectiveness of themethod is embodied in that by using low-cost and feasible cinchona quaternary ammonium salt being the phase-transfer catalyst, and through the phase-transfer catalysis, the asymmetric alpha-difluoromethylation of beta-ketoester compounds is successfully achieved for the first time. The invention provides a novel and effective approach for synthesizing the alpha-difluoromethyl-beta-ketoester compound having optical activities.