113 results about "Trifluoroacetic anhydride" patented technology

Provided is a novel method of cleaning a chemical vapor deposition processing chamber having deposits on an inner surface thereof is provided. The process involves forming a plasma from one or more gases comprising a fluorine-containing but otherwise halogen-free non-global-warming compound, and contacting active species generated in the plasma with the inner surface of the chamber, with the proviso that the non-global-warming compound is not trifluoroacetic anhydride. Also provided is a method of etching a layer on a silicon wafer. The method involves the steps of: (a) introducing a silicon wafer into a processing chamber, the silicon wafer comprising a layer to be etched; and (b) forming a plasma from one or more gases comprising a fluorine-containing but otherwise halogen-free non-global-warming compound. Active species generated in the plasma are contacted with the silicon wafer, thereby etching the layer, with the proviso that the non-global-warming compound is not trifluoroacetic anhydride. The chemistries in accordance with the invention provide environmentally benign alternatives to the conventionally used global-warming chemistries for chamber cleaning and semiconductor etching processes.

The invention relates to a method for synthesizing a beta-lactamase inhibitor Avibactam and belongs to the technical field of preparation of beta-lactamase inhibitors. The method disclosed by the invention comprises the following steps: (1) taking a compound 2 as a raw material, and reacting with R<1>NH2 so as to produce a compound 3; (2) enabling the compound 3 and a biocatalyst to produce a compound 4 in an organic solvent in the presence of glucose or sucrose; (3) enabling the compound 4 to react with trifluoroacetic anhydride so as to obtain a compound 5; (4) enabling the compound 5 to react with R<2>ONH2 so as to produce a compound 6; (5) hydrolyzing the compound 6 under alkaline conditions so as to produce a compound 7; (6) enabling the compound 7 to react with triphosgene so as to produce a compound 8; (7) enabling the compound 8 to react with ammonium formate in the presence of a catalyst so as to produce a compound 9 in the organic solvent, wherein the catalyst is a Pd/C system; and (8) enabling the compound 9 to react with a sulfonating agent, thereby obtaining the product 1. The method disclosed by the invention is stable in process, high in yield, simple and safe in operation and low in production cost.

The invention discloses a preparation method for vinorelbine tartrate; the preparation method comprises the following steps of: taking tartrate vinblastine as a starting material; using ammonia water for dissociating the starting material, reacting the dissociated starting material with the metachloroperbenzoic acid so as to obtain vinblastine-N oxide, then reacting the vinblastine-N oxide with vindoline and trifluoroacetic anhydride, carrying out the reduction through sodium borohydride so as to obtain dehydrated vinorelbine, treating the dehydrated vinorelbine so as to obtain vinorelbine, and finally salifying the vinorelbine with tartaric acid so as to obtain the vinorelbine tartrate. The preparation method has the advantages of low cost, few side reaction, easily controlled operation process, higher yield and product purity and wide industrialized application prospect.

The invention discloses a high selectivity method for synthesizing moxifloxacin. The method comprises the following steps of: reacting boric anhydride with trifluoro acetic anhydride to obtain a chelant; reacting 1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxo-3-quinolinecarboxylic acid ethyl ester with the chelant, cooling to room temperature, adding ice water, performing suction filtration, and washing a filter cake with water until neutrality to obtain a 1-ethyl-7-chloro-6-fluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid methyl ester trifluoroacetic anhydride boronized chelate; and reacting the 1-ethyl-7-chloro-6-fluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid methyl ester trifluoroacetic anhydride boronized chelate with (S,S)-2,8-diazabicyclo[4,3,0]nonane to obtain a 1-cyclopropyl-6-fluoro-7-([S,S]-2,8-diazabicyclo[4,3,0]nonane-8-methoxy-4-oxo-1,4-dihydro-3-quinolinecarboxylic acid ethyl ester trifluoroacetic anhydride boronized chelate, recycling a solvent under reduced pressure, adding alkali, refluxing, discoloring, filtering, freezing, performing suction filtration, and drying a filter cake. The method is simple, mild in conditions, and high in selectivity, avoids difficultly separated impurities, is high in reaction yield and product purity, and is suitable for industrial production.

The invention discloses a fast detection method for detecting anionic surface active agent of sulfuric acids, which comprises: a potassium iodide is mixed with a sulfuric acid negative ion surface active agent by a molar ratio of 1:1-10:1, then N and N-dimethyl formamide having the amount of 5 to 20ml/mol of potassium iodide are added into the mixture, the mixture is agitated to reach complete dissolution, then trifluoroacetic anhydride with the molar ratio one to ten times the amount of potassium iodide is added into the solution, the solution turns into red and is taken for implementing the conventional gas phase chromatography-mass spectrum detection and then data processing analysis when the color stops darkening, thereby obtaining the detecting result. The detection method has advantages of fast and simple reaction process and easy control of conditions, and makes up defects that the traditional detection method has false positive easily and can not ensure detection results and has high requirements on sample pre-processing, and the method is particularly suitable for qualitative and quantitative analysis of all components in complex compounds such as anionic surface active agent.

The invention relates to [(10S)-9,10-dihydroartemisinine-10-oxyl]benzaldehyde semicarbazones (sulfur) series substances and provides a structure, a preparation method and application of a novel artemisinine 10-locus derivative. The structural formula of the [(10S)-9,10-dihydroartemisinine-10-oxyl]benzaldehyde semicarbazones (sulfur) series substance is shown in a formula I. The invention also relates to pharmaceutically-acceptable slats, a solvate, an optical isomer or a polymorphic substance of the [(10S)-9,10-dihydroartemisinine-10-oxyl]benzaldehyde semicarbazones (sulfur) series substances and a medicinal composition by taking the compounds as active components. As novel antimalarial agents, anti-tumor agents and antifungal agents, the compounds can be used for treating or preventing malaria, mycotic infection, malignant tumor and the like. The compounds can be prepared by reacting dihydroartemisinine as an initial raw material with trifluoroacetic anhydride/triethylamine to obtain 10(R)-trifluoro-acetoxyl-9,10-dihydroartemisinine, directly reacting the 10(R)-trifluoro-acetoxyl-9,10-dihydroartemisinine with hydroxy benzaldehyde without separation to obtain (10S)-9,10-dihydroartemisinine-10-oxyl]benzaldehyde, and reacting the (10S)-9,10-dihydroartemisinine-10-oxyl]benzaldehyde with the substituted amino (sulfur) urea compounds in acid catalysts and alcohol solvents to obtain target compounds.

The invention discloses a preparation method of a thioether compound and a product of the sulfoether compound. The method comprises the following steps: adding a sulfoxide compound into acetonitrile or dichloromethane under the protection of gas which does not react with a substrate, cooling the mixture, then adding trifluoromethanesulfonic anhydride or trifluoroacetic anhydride, adding an arylphenol compound, keeping the temperature and stirring for 2 to 4 hours, adding potassium phosphate, heating to 65 to 75 DEG C, stirring for 20 to 28 hours, and carrying out extraction and concentration chromatography to obtain a target product. The method for preparing the sulfoether compound has the characteristics of simplicity, efficiency, mildness and economy.

The invention discloses a high performance liquid chromatography detection method for the abamectin content in edible vegetable oil. The method comprises the steps that a sample is subjected to vortex oscillation extraction through methanol, purified with an ODS C18 solid-phase extraction column, subjected to derivatization through N-methylimidazole and trifluoroacetic anhydride and lastly determined through a liquid chromatography-fluorescence method. According to the method, few reagents are adopted, and the cost is reduced; a sample pretreatment method is simple, the purification effect is good, maintenance of instruments in the using process is reduced, and the technical problems that when a liquid chromatography-ultraviolet detector is used, the sensitivity is too low, and matrix interference is serious are solved; a determined result is accurate and good in repeatability, the detection specificity and sensitivity are high, and a reference is provided for detection of the abamectin content in the edible vegetable oil.

The invention discloses a synthetic method of a compound, which belongs to the technical field of organic synthesis. A synthetic method of 3,5-2-fluoro-(trifluoromethyl)benzophenone comprises the following steps: putting solvents and iodine into a four-port reaction kettle, and under the protection of nitrogen, putting magnesium chips and a small amount of bromoethane into the reaction kettle to carry out initiation reaction, wherein the reaction time is controlled in 15min; dropwise adding 3,5-difluorobromobenzene into the reaction kettle at 30-40 DEG C; after the adding step is completed, stirring the obtained mixture for 2h at 35 DEG C so as to obtain a Grignard reagent; slowly dropwise adding the obtained Grignard reagent into a trifluoroacetic anhydride solvent solution at 20-30 DEG C; and after the adding step is completed, carrying out thermal reaction for 1-1.5h at 25 DEG C; slowly adding the obtained reaction liquid into ice water, separating out an organic layer, extracting a water layer by using ethyl acetate, combining with the organic layer, carrying out water washing, drying and solvent recovery on the organic layer so as to obtain a coarse product, and carrying out rectification on the coarse product so as to obtain a pure product. The synthetic method disclosed by the invention is low in raw material cost, simple in process condition, easy to operate, moderate to the environment, and high in product yield.

The invention discloses a method for preparing 3-trifluoromethyl pyrrole boric acid, belonging to the technical field of organic chemical synthesis. The method is characterized by comprising the following steps: (I) with trifluoroacetic anhydride as a start raw material, generating 4-ethoxy-3-alkenyl trifluoroacetyl ketone through reaction between the trifluoroacetic anhydride and ethyl vinyl ether; (II) performing heating reflux of 4-ethoxy-3-alkenyl trifluoroacetyl ketone and hydrazine dihydrochloride in an ethanol solution to obtain 3-trifluoromethyl pyrrole; and (III) performing functional group conversion of 3-trifluoromethyl pyrrole to generate 1-methyl-3-trifluoromethyl-5-pyrrole boric acid, N-tert-butyl acyl-3-trifluoromethyl-5-pyrrole boric acid and 1-methyl-3-trifluoromethyl-4-pyrrole boric acid respectively. The method has the beneficial effects that the generated target compound has good purity and stable properties, the method is simple and easy to operate, and the preparation scale is easy to enlarge to realize industrial production.

The invention discloses a sulfonium sulfonate salt photoacid generator synthesized from beta-cineole, and a synthesis method thereof, and belongs to the field of chemical synthesis and photoetching materials. The structural general formula of the photoacid generator is shown in the description; and in the formula, R1 is one of three formulas also shown in the description, and R2 is one of an alkylgroup, a naphthenic base, an ester group-containing alkyl group and a fluorine-containing alkyl group. The synthesis method of the photoacid generator comprises the following steps: reacting beta-cineole with a sulfonate compound to obtain an intermediate; and reacting the intermediate with (cyclohexyl-1,5-dienyloxy)-trimethyl-silane, tetramethylene sulfoxide and trifluoroacetic anhydride to obtain the sulfonium sulfonate photoacid generator. The beta-cineole used as the raw material has a high molecular weight, and the photoacid generator formed by the beta-cineole also has a high molecularweight, so that the diffusion of the photoacid generator can be reduced, and the improvement of the edge roughness, the reduction of the line width roughness and the improvement of the resolution ratio are facilitated.

The invention discloses a method and device for preparing heptafluoroisobutyronitrile, wherein the method comprises the steps: adding methyl heptafluoroisobutyrate into a reaction kettle, adding an alcoholic solution of ammonia, and controlling the reaction temperature to be lower than 0 DEG C; carrying out a reaction for 2-5 h, heating to 60 DEG C, finishing the reaction when the content of methyl heptafluoroisobutyrate in a reaction solution is less than 0.1%, removing a methanol solvent by vacuum distillation, and removing the vacuum when the content of methanol in the reaction solution inthe reaction kettle is less than 1%; and adding a dimethylformamide/pyridine solvent into the reaction system, controlling the reaction temperature to be lower than 0 DEG C, adding a dehydrating agenttrifluoroacetic anhydride, and collecting heptafluoroisobutyronitrile gas. According to the method, an intermediate heptafluoroisobutyrylamide synthesis step and a step device for preparing heptafluoroisobutyronitrile by dehydrating heptafluoroisobutyrylamide are integrated; transfer of an intermediate heptafluoroisobutyramide is not needed and water washing, extraction, recrystallization and other operations are avoided, so the heptafluoroisobutyronitrile is directly synthesized, the equipment investment is greatly reduced, the operation process is simplified, and the method is suitable forindustrial production.

The invention discloses a synthetic method for diaryl selenide, and belongs to the technical field of organic synthesis. According to the method, aryl benzyl selenium oxide or 2-pyridyl benzyl selenium oxide and a phenolic compound are dissolved in anhydrous dichloromethane under a nitrogen atmosphere, and an activator trifluoroacetic anhydride is added at room temperature to obtain a reaction system; the reaction system is sealed in a nitrogen atmosphere, a reaction is performed under a stirring condition, a saturated sodium hydrogen carbonate solution is added for quenching the reaction, dichloromethane is adopted for washing, then a saturated salt solution is adopted for washing, phase separation is carried out, an organic phase is subjected to drying, filtration and reduced pressure distillation to remove a solvent, and through slica column chromatography, the diaryl selenide is obtained. The method has the advantages that no transition metal catalysis exists, the reaction conditions are mild, the functional group compatibility is excellent, the yield is generally high, and environmental friendliness is achieved.

The invention provides a synthetic method for a trifluoromethyl methylation arene. The trifluoromethyl methylation arene is prepared by reacting a halogenated arene, copper powder, elemental iodine and trifluoroacetic anhydride in an organic solvent under an inert atmosphere protection state. The method has the advantages of being simple and efficient, cheap in raw materials, low in synthetic cost, high in universality and repeatability, and the like, and can be popularized and applied to the fields of the synthesis of trifluoromethyl methylation aromatic derivatives.

The invention discloses a diarylo[d,f]oxacycloheptane-3-ketone compound and a synthesis method thereof, relating to an oxacycloheptane-3-ketone compound and a synthesis method thereof. The invention aims to solve the problems that in the prior art, the diarylo[d,f]oxacycloheptane-3-ketone compound is difficult to synthesize, the pollution is serious and the industrial production can not be realized. The structural formula of the diarylo[d,f]oxacycloheptane-3-ketone compound is shown in the specification. The method takes 2-phenylphenoxyacetic acid derivatives or 2-naphthphenoxyacetic acid derivatives as raw materials, and comprises the following steps of: carrying out reaction between trifluoroacetic anhydride and lewis acid as catalysts in an organic solvent; pouring ice water and layering; adjusting the pH value of the organic layer to 8-9 by the aqueous solution of sodium carbonate; washing the organic layer without a water layer by saturated salt water; and concentrating to obtain a solid crude product, and recrystallizing to obtain the diarylo[d,f]oxacycloheptane-3-ketone compound. The method disclosed by the invention is mainly used for synthesizing the diarylo[d,f]oxacycloheptane-3-ketone compound.

The invention discloses a preparation method of a prucalopride intermediate. The preparation method comprises the following steps: step a, protecting t amino group of a compound I by using trifluoroacetic anhydride to obtain a compound II; step b, under the protection of nitrogen gas, enabling the compound II, chloroacetyl chloride, anhydrous aluminium chloride, nitrobenzene and a halocarbon solvent to react to obtain a compound III; step c, enabling the compound III, an alcohol solvent and sodium acetate to have a reflux reaction to obtain a compound IV; step d, enabling the compound IV, the alcohol solvent, raney nickel and nitrogen with the pressure of 3.0Mpa to react to obtain a compound V; step e, enabling the compound V and N-chloro-succinimide to have a substitution reaction to obtain a compound VI; step f, removing an amino protective group from the compound VI to obtain a compound VII. The method disclosed by the invention has the advantages that initial raw materials are easily available, is simple and convenient to operate, is relatively mild in reaction condition, is capable of avoiding the use of heavy metal reagents and high-toxicity reagents, is high in yield and is quite suitable for large-scale industrial production.

The invention discloses a method for synthesizing an optically active benzo carboxylic acid ester compound through an asymmetric addition reaction, and belongs to the technical field of asymmetric synthesis in organic chemistry. Tert-leucine is used as an initial raw material and reacts with trifluoroacetic anhydride to generate a 2-trifluoroalkyl oxazole-5 (2H) ketone intermediate product, and then in the presence of a chiral bifunctional tertiary amine urea catalyst, the optical benzo carboxylic acid ester compound is synthesized through asymmetric addition reaction and one-pot two-step synthesis. The method has the advantages that the reaction raw materials are easy to obtain, the catalyst is simple in structure, the catalytic efficiency is high, the reaction conditions are mild, post-treatment is simple, and the high-optical-activity benzo carboxylic acid ester compound is obtained.

The invention discloses fluorine-contained hydrophobic oil-proof modified nanocellulose for food packaging paper and a preparation method of the nanocellulose and belongs to the technical field of functional materials. According to the preparation method, firstly, oxidized nanocellulose is diluted into a nanocellulose water suspension with the concentration of 1-1.5%, then evaporation is performedto obtain gel nanocellulose, then trifluoroacetic anhydride and 2,2-difluoroethylamine are sequentially used for modifying the nanocellulose, and the fluorine-contained hydrophobic oil-proof modifiednanocellulose is obtained. The fluorine-contained hydrophobic oil-proof modified nanocellulose has good water resistance and film-forming performance; after the nanocellulose is spread on the surfaceof the food packaging paper, a uniform film can be formed to effectively prevent permeation of water vapor and oxygen, and therefore the shelf life of food is prolonged; and besides, since the nanocellulose has a great specific surface area and contains abundant hydroxide radicals, the nanocellulose can be tightly combined with fibers, the binding force between the fibers and the strength of thepaper are improved, and the reliability of the food packaging paper in use is improved.

The invention relates to a preparation method of (1S, 3S, 5S)-3-(amidogen carbonyl)-2- azabicyalo [3.1.0] hexane-2-tert-butyl formate. The preparation method comprises the following steps that (1), Boc-L-pyroglutamic acid methyl ester is restored through lithium triethylborohydride and then dewatered through trifluoroacetic anhydride to obtain (S)-1-N-tert-butyloxycarbonyl-2,3-dihydro-2-pyrrole ethyl formate; (2), DIPEA is added in the hydrolysis reaction of (S)-1-N-tert-butyloxycarbonyl-2,3-dihydro-2-pyrrole ethyl formate under a alkaline condition, then salifying is conducted, and (S)-1-N-tert-butyloxycarbonyl-2,3-dihydro-2-pyrrole formic acid N, N-diisopropyl ethylamine salt is obtained; (3), (S)-1-N-tert-butyloxycarbonyl-2,3-dihydro-2-pyrrole formic acid N and N-diisopropyl ethylamine salt obtained in the step (2) are subjected to amidating, and (S)-1-N- tert-butyloxycarbonyl-2,3-dihydro-2-pyrrole formamide is obtained; and (4), (S)-1-N-tert-butyloxycarbonyl-2,3-dihydro-2-pyrrole formamide is catalyzed through a chirality nickel catalyst and subjected to a ciprofloxacin reaction, and a target material with single configuration, namely (1S, 3S, 5S)-3-(amidogen carbonyl)-2-azabicyalo [3.1.0] hexane-2-tert-butyl formate (SM1), is obtained.

The invention belongs to the field of biological medicine, and discloses a nitroreductase-responsive diagnosis and treatment integrated probe and a preparation method and application thereof. The structural general formula of the diagnosis and treatment integrated probe is described in the specification. The specific preparation method comprises the following steps: reacting hydrogen peroxide with trifluoroacetic anhydride in an organic solvent, then adding a near-infrared fluorescent dye for continuous reaction, and after the reaction is finished, separating and purifying to obtain the diagnosis and treatment integrated probe. The diagnosis and treatment integrated probe can show fluorescence enhanced response to nitroreductase in a tumor microenvironment, and is used for nitroreductase and living tumor imaging; meanwhile, the diagnosis and treatment integrated probe generates active oxygen under laser irradiation and is used for photodynamic therapy of tumors. The diagnosis and treatment integrated probe has high biological safety, the preparation method is easy and convenient to operate, low in cost and easy to popularize, and the diagnosis and treatment integrated probe has potential application value in the aspects of early diagnosis and treatment of malignant tumors.

The invention relates to a rabeprazole preparation method. The method concretely comprises the following steps: dissolving 2,3-dimethyl-4-nitropyridin-N-oxide in dichloromethane, adding trifluoroacetic anhydride in a dropwise manner, distilling off excess trifluoroacetic anhydride, adding dichloromethane, adding triethylamine and 2-mercaptobenzimidazole, adding ethanol and water, stirring for 30min, filtering to obtain 2-[[(3-methyl-4-nitro-2-pyridyl)methyl]thio]-1H-benzimidazole, carrying out column chromatography on the obtained residue to obtain 2-[[(3-methyl-4-(3-methoxypropanolato)-2-pyridyl)methyl]thio]-1H-benzimidazole, adding a dichloromethane solution of m-CPBA, adjusting the pH value to 13.0 by using 10% sodium hydroxide, separating out the obtained water layer, and adding dichloromethane to obtain the product rabeprazole. The rabeprazole preparation method is simple, and the quality of the product is good.