512 results about "Methanesulfonic acid" patented technology

The invention provides a metallized film for a capacitor, a preparation method of the metallized film and the capacitor, and relates to the technical field of capacitor manufacturing. The preparation method of the metallized film comprises the following steps: preparing an inorganic reinforcing material from raw materials including 1, 4-phthalaldehyde, zirconium diboride and tetraethoxysilane; the preparation method comprises the following steps: preparing a modified polypropylene material from raw materials including 4, 4 '-diaminobiphenyl, triphenyl phosphate, an ethylene-1-octylene copolymer, polyethylene and polypropylene; raw materials including polyvinyl alcohol, a silane coupling agent, N-hydroxynaphthalimide trifluoromethanesulfonic acid, an inorganic reinforcing material and a modified polypropylene material are subjected to melt mixing, casting piece forming and two-way stretching, and a base film is obtained; applying a polyester coating on the base film, and carrying out irradiation treatment on the base film by adopting an electron beam and an ultraviolet light source to obtain a modified base film; a metal layer is formed on the modified base film through vacuum evaporation, and the metallized film is obtained. The metallized film obtained by the invention has good thermal stability and mechanical properties.

The present invention relates to a method for manufacturing a hydrogel. The method comprises the steps of providing an agarose and providing an aqueous solution of a salt comprising Zn2+, wherein the salt is selected from zinc methanesulfonate, zinc acetate, zinc chloride, or a combination thereof. The method further comprises combining the agarose and the aqueous solution to form a mixture and forming a hydrogel from said mixture. The present invention also relates to a hydrogel, an electrolyte comprising the hydrogel, and an energy storage device comprising the electrolyte.

The invention provides a low-temperature sodium ion electrolyte and a preparation method and application thereof, the low-temperature sodium ion electrolyte comprises a sodium salt, an organic solvent and an additive, the additive is triisopropyl silyl trifluoromethanesulfonate, and the sodium salt is sodium trifluoromethanesulfonate. Triisopropyl silyl trifluoromethanesulfonate molecules are used as an electrolyte additive for the low-temperature sodium ion electrolyte, so that further decomposition of sodium salt in the electrolyte can be effectively promoted, stable SEI containing more sodium fluoride is formed to promote mass transfer of sodium ions at low temperature, and finally, a sodium ion battery can effectively circulate at low temperature.

The invention provides a synthesis method of (3-hydroxyadamantane-1-methoxycarbonyl) difluoromethanesulfonate photoacid generator anions, and relates to a photoacid generator anion synthesis method of (3-hydroxyadamantane-1-methoxycarbonyl) difluoromethanesulfonate photoacid generator anions. The preparation method comprises the following steps: S1, uniformly mixing a solvent and difluorobromoacetic acid, then adding CDI, fully stirring, then adding 3-hydroxy-1-adamantane methanol, fully reacting, then adding bicarbonate, carrying out liquid separation to obtain an organic phase A, washing the organic phase A, and carrying out drying and spin-drying; s2, fully mixing the spin-dried substance with NaHCO3, Na2S2O4, acetonitrile and ultrapure water, then carrying out liquid separation to obtain an organic phase B, and carrying out drying and spin-drying on the organic phase B; and S3, dissolving the spin-dried substance in water, then adding an H2O2 solution, carrying out a full reaction, and then carrying out cooling and post-treatment so as to obtain the photoacid generator anions. According to the method, 3-hydroxy-1-adamantane methanol and difluorobromoacetic acid are used as reaction raw materials, esterification reaction is performed under the condition of adding CDI to obtain a first-step reaction intermediate, then acylation sulfonation and oxidation reaction are performed to obtain the target product photoacid generator anion, the reaction process is mild in condition, and the product purity is high.

The invention relates to a preparation method of rotigotine, which solves the technical problems of unreasonable reaction steps and higher production cost in the prior art, and comprises the following steps: carrying out chiral amination reduction reaction on 5-methoxy-2-tetralone, chiral phosphate, pinacol borane and p-methoxyaniline to obtain a compound 1; reacting the compound 1 with bromopropane to obtain a compound 2; reacting the compound 2 with ceric ammonium nitrate to obtain a compound 3; dissolving the compound 3 in hydrobromic acid, and reacting to obtain a compound 4; and carrying out a reaction on the compound 4 and 2-thiophene ethyl methanesulfonate to obtain a crude product rotigotine. The method can be applied to the field of preparation of rotigotine.

The invention discloses a synthesis process of chiral cyclic ether indole. The synthesis process comprises the following steps: reacting 4-bromobenzaldehyde with malonic acid under the catalysis of piperidine to generate olefin carboxylic acid CHP-1; carrying out condensation reaction to prepare CHP-2; under the catalysis of a copper reagent, carrying out Michael addition reaction to obtain CHP-3; preparing a chiral alcohol intermediate CHP-4 through a reduction reaction; trifluoromethanesulfonic acid is used, and a chiral ether intermediate CHP-5 is prepared through ring closing; reacting with protected hydrazine by using a copper ion catalyst to obtain an intermediate CHP-6; the method comprises the following steps: by taking alcohol as a solvent, adding strong acid, and removing a protecting group of hydrazine to obtain an intermediate CHP-7; and carrying out ring closing by taking lewis acid as a catalyst to obtain an indole product CHP-8. The use of a noble metal catalyst palladium is avoided, and the cost is greatly reduced. The chiral center is directly constructed through a chemical method, and SFC is not needed for resolution, so that the cost is remarkably reduced, and industrial production is successfully realized.

The invention belongs to the field of light-emitting diodes, and discloses a preparation method of a blue-light perovskite thin film containing a sulfonate additive and a light-emitting device of the blue-light perovskite thin film. According to the technical scheme, sulfonate functional additives (such as methyl methanesulfonate and the like) with the addition amount being 0.5%-1.5% of the molar weight of lead ions are introduced into a full-inorganic CsPb (BrxCl1-x) 3 perovskite precursor solution, the molar ratio of chlorine to bromine is controlled to be 0.5: 1-2: 1, and the thin film is formed through spin coating and annealing treatment at the temperature of 110-130 DEG C. Sulfonate groups in additive molecules are effectively coordinated with uncoordinated lead ions in perovskite crystals, so that defects of grain boundaries and surfaces are passivated, and a non-radiative recombination center is inhibited; meanwhile, accurate adjustment of the wavelength of the blue light is realized through regulation and control of the halogen proportion. A blue light perovskite light-emitting diode device prepared based on the modified thin film realizes high-brightness, high-efficiency and wavelength-adjustable blue light emission.

The invention relates to the technical field of pharmaceutical preparations, and discloses a mild photo-thermal microneedle patch and a preparation method and application thereof, and the mild photo-thermal microneedle patch comprises a substrate and needle tips arranged on the substrate in an array; the substrate is prepared from the following raw materials in parts by weight: 400 to 500 parts of N-isopropylacrylamide, 30.5 to 40.5 parts of acrylamide, 4 to 5 parts of polydopamine nanoparticles, 10 to 30 parts of N, N-methylene bisacrylamide, 100 to 200 parts of sodium alginate, 6.2 to 9.3 parts of tetramethylethylenediamine and 8 to 12 parts of potassium persulfate; the needle tip is prepared from the following raw materials in parts by weight: 0.1 to 0.5 part of methacrylated gelatin, 0.2 to 0.6 part of deferoxamine mesylate, 0.8 to 1.2 parts of a photoinitiator and 33.6 to 56 parts of polyethylene glycol diacrylate. The mild photo-thermal microneedle patch can realize photo-thermal sterilization under near-infrared irradiation, and also can promote skin repair and regeneration.

This invention belongs to the field of chemical synthesis and relates to a method for achieving deuterated methylation of a nucleophile. The invention provides a deuterated methylating reagent, which is obtained by reacting formic acid with deuterated methanol under acidic conditions, followed by a second reaction with thiaanthracite and trifluoromethanesulfonic acid. The nucleophile is then reacted with the deuterated methylating reagent described in claim 1, a base, and a solvent to obtain the deuterated methylated product. This invention also provides a method for achieving deuterated methylation of a nucleophile, which involves dissolving the nucleophile and 5-deuterated methyl-5H-thiophene-5-onium trifluoromethanesulfonate in a suitable solvent, adding a base, and then performing the deuterated methylation reaction at room temperature. In the method provided by this invention, the yield of the product after nucleophile methylation can reach 52% to 95%.

The invention discloses a preparation method of deuterated methylamine hydrochloride and a solid-phase continuous flow synthesis system, and relates to the technical field of deuterated synthesis. The preparation method comprises the following steps: adding out-of-phase polykadexide into methyl trifluoromethanesulfonate and 1, 2-dichloroethane for heating reaction, then adding methanol for quenching reaction, washing and drying to obtain an out-of-phase polykadexide type methyl reagent; the method comprises the following steps: adding a heterophase polysulfide-type methyl reagent into a mixed solvent of a polar solvent and heavy water, and carrying out alkali treatment to complete deuteration conversion, so as to obtain a heterophase polysulfide-type deuterated methyl reagent; the preparation method comprises the following steps: dissolving o-phenylsuccinimide in acetonitrile, and adding a heterophase polysulfide deuterium methyl reagent and inorganic alkali to react, so as to obtain N-(1, 1, 1-trideuterium methyl) benzo-succinimide; the preparation method comprises the following steps: hydrolyzing N-(1, 1, 1-trideuterium methyl) benzo-succinimide and hydrochloric acid in an aqueous solvent to obtain deuterated methylamine hydrochloride. The preparation method is simple, the deuterium source is cheap, the atom utilization rate is high, the deuteration rate is high, and the production cost is low.

Provided is a method for producing a protected glycoside derivative, including reacting a sugar in which all hydroxyl groups of the sugar are protected by protective groups and protective groups of a hydroxyl group at a 1-position and a hydroxyl group at a 2-position are acyl groups, with a phenolic compound in the presence of at least one catalyst selected from the group consisting of trifluoromethanesulfonic acid and copper (II) trifluoromethanesulfonate, in which the phenolic compound is bonded to an anomeric position of the sugar and other hydroxyl groups of the sugar are protected.

The invention discloses a wide-voltage wide-temperature-range sodium-ion battery electrolyte and a preparation method and application thereof, and belongs to the technical field of sodium-ion battery electrolytes.The wide-voltage wide-temperature-range sodium-ion battery electrolyte comprises sodium salt, an organic solvent and an additive, the organic solvent is selected from one or more of ethylene carbonate, propylene carbonate, ethyl methyl carbonate, dimethyl carbonate, diethyl carbonate, ethylene glycol dimethyl ether, diethylene glycol dimethyl ether and triethylene glycol dimethyl ether, and the additive is selected from one or more of fluoroethylene carbonate, allyl-1, 3-propane sultone, 1, 3-propylene sultone, 1, 3-propylene sultone and 1, 3-propylene sultone. The additive is one or more of 1, 3-propyl sultone, methylene methane disulfonate, ethylene sulfate, trifluoromethanesulfonic anhydride, pentaerythritol bicyclic sulfate, tri (trimethylsilane) phosphate, tri (trimethylsilane) phosphite, tri (trimethylsilane) borate, acesulfame sodium and aluminum trifluoromethanesulfonate, and the additive is one or more of 2, 3-propylene sultone, methylene methane disulfonate, ethylene sulfate, trifluoromethanesulfonic anhydride, pentaerythritol dicyclosulfate, tri (trimethylsilane) phosphate, tri (trimethylsilane) phosphite, tri (trimethylsilane) borate, tri (trimethylsilane) phosphate and tri (trimethylsilane) borate. The electrolyte provided by the invention not only keeps high coulombic efficiency at low temperature, but also has good cycle stability at high temperature.

The invention discloses an electrolyte containing a redox medium as well as preparation and application of the electrolyte. The positive electrode electrolyte and the negative electrode electrolyte comprise tetravalent or trivalent vanadium ions, mixed acid, an iron ion additive and water, the iron ion additive is composed of iron phthalocyanine and a second iron-containing compound, and the second iron-containing compound comprises at least one of ferric acetylacetonate, heme iron and iron trifluoromethanesulfonate. The preparation method comprises the following steps: activating vanadium pentoxide in mixed acid, adding water to obtain a mixed solution, and adding a reducing agent into the mixed solution to react to obtain an initial mother solution; adding an iron ion additive into the initial mother solution, and uniformly mixing to obtain a positive electrode electrolyte; and electrolyzing the initial mother liquor to obtain electrolyte containing trivalent vanadium ions, adding an iron ion additive into the electrolyte, and uniformly mixing to obtain the negative electrode electrolyte. The charge-discharge polarization is reduced by using a small amount of iron ion additive containing iron phthalocyanine; the capacity fading caused by pentavalent vanadium precipitation is released; and the energy efficiency and the cycling stability of the battery are improved.

The invention discloses a method for preparing polycaprolactone by ring-opening polymerization, and aims to provide a method for preparing polycaprolactone by ring-opening polymerization with the advantages of high catalytic activity, mild conditions, simple process and the like. The method uses ε-caprolactone as a monomer and trifluoromethanesulfonate metal as a catalyst, and prepares polycaprolactone by a bulk polymerization method under the condition that the reaction temperature is 100-160 DEG C. The invention uses trifluoromethanesulfonate metal as a catalyst for the polymerization preparation of ε-caprolactone, and belongs to the technical field of polymer organic synthesis.

The invention provides a method for rapidly synthesizing thiocyano-substituted formanilide, which belongs to the technical field of organic chemical preparation, and comprises the following steps: taking alpha-aminoketone and potassium thiocyanate as initial raw materials, sealing in an oil bath pan under the condition of a copper catalyst, an oxidizing agent and an organic solvent, stirring at 80 DEG C, and heating to react for 24 hours, thereby obtaining the thiocyano-substituted formanilide. The copper catalyst comprises any one of copper chloride, copper acetate, copper sulfate, copper acetylacetonate and copper trifluoromethanesulfonate, and the oxidizing agent comprises one of iodobenzene diacetic acid, potassium persulfate, di-tert-butyl peroxide and tert-butyl hydroperoxide. The method overcomes the problems of many reaction steps, low synthesis efficiency and the like in the prior art, and has the advantages of easily available raw materials, simple operation and the like.

The invention relates to the technical field of fine chemical engineering, in particular to a preparation method of methyl trifluoromethanesulfonate, which comprises the following steps: adding trifluoromethanesulfonic acid into a reaction kettle, adding a catalyst 4-dimethylaminopyridine under the conditions of cooling and stirring, and continuously stirring to obtain a pre-reaction system; raising the temperature, dropwise adding dimethyl carbonate, and after dropwise adding is completed, continuously reacting to obtain a mixed solution containing a product methyl trifluoromethanesulfonate; standing and layering to obtain an organic phase and a water phase; taking an organic phase, rectifying at normal pressure, and collecting fractions to obtain a product methyl trifluoromethanesulfonate; and taking a water phase, carrying out reduced pressure distillation, removing water, and recovering the catalyst. 4-dimethylaminopyridine is used as a catalyst to catalyze trifluoromethanesulfonic acid to react with dimethyl carbonate to prepare methyl trifluoromethanesulfonate. Compared with the prior art, the method has the advantages that steps and devices are simple, the used catalyst is low in toxicity and small in dosage, no organic solvent is used, and harm to human health is reduced.

The invention relates to a zinc negative electrode modifier with a zinc-philic-hydrophobic double-interface protective layer, a modification method and application of the zinc negative electrode modifier, and belongs to the technical field of zinc ion batteries. According to the zinc ion battery negative electrode modification method, absolute ethyl alcohol, deionized water, zinc-philic or hydrophobic silane and zinc trifluoromethanesulfonate are uniformly mixed to obtain a modification solution, and the volume ratio of absolute ethyl alcohol to deionized water to silane is 90: 5: 5; the concentration of the zinc trifluoromethanesulfonate is 0.05 mol L <-1 > to 0.5 mol L <-1 >; the zinc-philic modification liquid and the hydrophobic modification liquid are sequentially sprayed to the surface of the pretreated zinc negative electrode, and the power of a spraying device is 2-10 W; the spraying time is 0.2-5 s cm <-2 >, and after spraying is completed, drying is conducted at the room temperature, and curing is conducted in a high-temperature drying box. According to the modification method, the generation of zinc dendrites and the generation of a hydrogen evolution reaction are inhibited by combining the dual effects of adjusting the zinc ion flux by the inner-layer zinc-philic silane and adjusting a hydrated ion solvation structure by the outer-layer hydrophobic silane, and the electrochemical performance of the battery is improved.

The application belongs to the field of fine chemical industry and environmental protection, and particularly relates to a method for preparing metal triflate by using high gravity reaction. The method comprises the following steps: 1, using trifluoromethylsulfonyl chloride and anhydrous HF gas as raw materials to generate trifluoromethylsulfonyl fluoride gas; 2, performing gas-liquid contact reaction of the trifluoromethylsulfonyl fluoride gas with an alkali metal solution to obtain a mixed solution; 3, performing solid-liquid separation on the mixed solution by using a filter press, and the liquid phase is a triflate salt solution; 4, drying the triflate salt solution by using a spray dryer to obtain a solid-phase product triflate salt. The method uses trifluoromethylsulfonyl chloride and anhydrous HF as raw materials to replace triflic acid in the traditional method, and utilizes high gravity reaction, so that the production cost is greatly reduced. The process is simple, the obtained product triflate metal salt has low impurity content, is superior to the industry standard, the process is zero emission, and has good economic value and social value.

The invention belongs to the field of drug mutagenesis impurity detection and analysis, and relates to a method for detecting impurities of trifluoromethanesulfonate, in particular to a method for detecting impurities of methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate. Specifically, according to the detection method disclosed by the invention, tetrabutylammonium bromide is used as a derivatization reagent to derivatize trifluoromethanesulfonate, a corresponding derivative halogenated alkane is detected by GC-MS (Gas Chromatography-Mass Spectrometer), and then the content of trifluoromethanesulfonate is determined. The method provided by the invention solves the problem that the detection result may have false negative in the prior art, and has the advantages of high sensitivity, low detection limit, good repeatability and high accuracy, and all substances can be well separated.

The invention belongs to the technical field of polymer materials, and particularly relates to a conductive polymer material as well as a preparation method and application thereof. The conductive polymer material is prepared from the following components in parts by weight: 0.1 to 5 parts of ionic liquid, 0.1 to 10 parts of filler and 1 to 100 parts of polymer, the ionic liquid comprises at least one of organic salt and metal salt; the organic salt comprises at least one of p-toluenesulfonic acid triethylamine salt, p-toluenesulfonic acid tripropylamine salt, trifluoromethanesulfonic acid triethylamine salt and trifluoromethanesulfonic acid tripropylamine salt; the metal salt comprises at least one of potassium trifluoromethanesulfonate and sodium trifluoromethanesulfonate. The conductive polymer material prepared by the invention has the advantages of excellent conductivity, high transparency, good water resistance, good mechanical properties, good environmental stability, strong thermal stability and strong self-repairing ability.

The application discloses a triazine ring synthesis method, and belongs to the technical field of medical intermediate synthesis. The method is characterized in that 2-methylaminothiourea and dimethyl oxalate are used as raw materials, a nanometer catalyst of scandium triflate (Sc(OTf)3) or ytterbium triflate (Yb(OTf)3) is loaded on magnetic Fe3O4@SiO2, a cyclization reaction is carried out in an organic solvent, the catalyst is separated and recovered through an external magnetic field after the reaction is completed, and high-purity triazine rings are obtained through acidification, crystallization and drying of the reaction liquid. The catalyst has the advantages of high specific surface area, high catalytic activity, easy magnetic separation and recovery, and can be reused more than 6 times. The product yield can reach 93% to 96%, and the purity is greater than or equal to 99.6%. The method realizes green, efficient and low-cost synthesis of triazine rings.

The invention provides a purification method of a naphthalimide high-purity electronic-grade photoacid generator. The method solves the problem that photo-acid cannot be purified by traditional recrystallization or directly through ion exchange columns and other methods. The method comprises the following steps: firstly synthesizing and preparing 1, 3-diketone-2-hydroxy-6-(1-hexyne) benzisoquinoline, then reacting with triethylamine and trifluoromethylsulfonyl chloride to generate a crude product 1, 3-diketone-2-(1, 1, 1-trifluoromethyl) methanesulfonic ester-6-(1-hexyne) benzisoquinoline, removing impurities from normal hexane to obtain a pure product, sublimating the material into a gas phase by using a quartz vacuum sublimation instrument, and purifying to obtain the 1, 3-diketone-2-(1, 1, 1-trifluoromethyl) methanesulfonic ester-6-(1-hexyne) benzisoquinoline. And then passing through Pure MTS9500 amino phosphonic acid type chelating resin, and finally cooling in a quartz tube to obtain the high-purity electronic-grade photoacid generator. According to the invention, the stability is high, the metal ion content is low, the purification process is convenient to process, the product is used as a photoresist-level core main material, the product is widely applied in the fields of semiconductor photoresist, other imaging systems, photocureable coatings and the like, the market scale is continuously expanded, and the product is an indispensable key material in semiconductor manufacturing and other related fields.

The invention discloses a 3-imido-4, 5-diaryl boron oxygen heterocyclic ring onium salt derivative as well as a preparation method and application of the 3-imido-4, 5-diaryl boron oxygen heterocyclic ring onium salt derivative. The 3-imido-4, 5-diaryl boron oxygen heterocycle onium salt derivative is prepared by taking acetylenic ketone potassium fluoborate, organic amine and 2-(trimethylsilyl) phenyl trifluoromethanesulfonate as raw materials, inorganic alkali and a weak acid buffer as accelerators and water and acetonitrile as solvents through a one-pot two-step reaction, and the compound can be used for preparing organic fluorescent materials, such as organic fluorescent materials, organic fluorescent materials, organic fluorescent materials, organic fluorescent materials, organic fluorescent materials and organic fluorescent materials. The compound has obvious aggregation-induced emission (AIE) property, high quantum yield and wider fluorescence range. The target product is prepared with high atom economy reaction and high yield, and the method has the advantages of cheap and easily available raw materials, mild reaction conditions, short synthetic route, wide universal range of substrates and the like.

The invention provides a photocatalytic method for degrading polystyrene into benzoic acid, which comprises the following steps: dissolving polystyrene in a mixed solvent containing acetonitrile and chlorobenzene, adding a catalyst FPQL-OMe and iron trifluoromethanesulfonate, and reacting under the conditions of oxygen atmosphere and illumination to generate benzoic acid, wherein the FPQL-OMe and the iron trifluoromethanesulfonate are synergistically used as a photocatalyst. The invention provides a method for photocatalytic degradation of polystyrene, which is mild in condition, rapid, efficient and high in selectivity, and particularly provides a photocatalytic method for degrading and converting polystyrene into benzoic acid at a relatively high yield.

The invention discloses a (2-phenoxyphenyl) phenyl sulfide compound and a synthesis method thereof, comprising the following steps: placing a 3-(phenylsulfinyl) tert-butyl propionate compound and a 2-(trimethylsilyl) phenyl trifluoromethanesulfonate compound in a 10 mL Shrek tube under an argon atmosphere, adding cesium fluoride and then adding a solvent, acetonitrile, and reacting at room temperature for 6 hours; after the reaction is completed, extraction, chromatographic separation, and drying are performed to obtain the target product. The present invention only uses cheap and readily available cesium fluoride as a fluorine source, and can efficiently obtain aryl sulfide compounds under mild conditions without the participation of a transition metal catalyst. The method provides a new approach for preparing various functionalized aryl sulfide compounds.

A quinazolinone catalyst with both N-N and C-C axis chirality and its synthesis method and application, its chemical structural formula is shown in Formula 4; Synthesis method: using indole-derived o-aminobenzamide and 1-naphthaldehyde derivative as raw materials, using molecular sieve as dehydrating agent, bromobenzene as reaction solvent, stirring for 4h under the catalysis of chiral phosphoric acid and 10°C, then adding ethyl acetate, 2,3-dichloro-5,6-dicyano-1,4-benzoquinone, stirring for 10h under room temperature, TLC tracking reaction to complete formula 3 compound; using formula 3 compound, phenylsilane, trifluoromethanesulfonic acid as raw materials, adding toluene, stirring reaction under 100°C, TLC tracking reaction to end to obtain formula 4 compound. The catalyst prepared by the present invention can be used as a chiral ligand in transition metal-catalyzed asymmetric allylation reaction, with excellent stereoselectivity control effect; the method has mild reaction conditions, low cost and high enantioselectivity.

The invention discloses a deuterium-labeled stable isotope compound of everolimus and a preparation method thereof, the preparation method comprising: heating and heat-insulating a toluene solution of rapamycin, then adding dropwise a toluene solution containing 2-(tert-butyldimethylsilyloxy)ethyl trifluoromethanesulfonate-d4 and an organic base, stirring and heat-insulating the reaction and then cooling naturally, and post-processing to obtain tert-butyldimethylsilyloxy-everolimus-d4, wherein the organic base is one of N,N-diisopropylethylamine, triethylamine, pyridine and 2,6-lutidine; at 0°C and under nitrogen protection, hydrochloric acid solution is added to a methanol solution of tert-butyldimethylsilyloxy-everolimus-d4, and the reaction solution is reprocessed after the stirring reaction to obtain the product. The present invention ensures that the product does not contain other impurities and non-isotopic everolimus that are difficult to separate by adding an organic base and 2-(tert-butyldimethylsilyloxy)ethyl trifluoromethanesulfonate-d4 simultaneously.

The invention provides a preparation method of trifluoromethanesulfonic acid ionic liquid. According to the preparation method, trifluoromethanesulfonic acid, pyrrole salt, pyridinium salt, pyrazine salt and the like are subjected to substitution reaction, static layering, organic phase water washing and organic phase drying to achieve the purpose of generating the trifluoromethanesulfonic acid ionic liquid. The prepared trifluoromethanesulfonic acid ionic liquid is high in purity, good in yield and suitable for large-scale industrial application. The method provided by the invention is green and environment-friendly, and does not use harsh reaction conditions and organic solutions; meanwhile, the cost is low, the yield is high, and the purity of a crude product can reach 99.95% or above after the crude product is purified; and the method has the advantages of less required equipment, small occupied area and low investment, and can realize industrial production.

The invention belongs to the field of pharmaceutical chemicals, and relates to a preparation method of an anti-influenza virus derivative intermediate. According to the invention, a compound (a) and a compound (b) are taken as initial raw materials, and an alcoholic hydroxyl group is directly converted into an active intermediate by utilizing trimethylsilyl trifluoromethanesulfonate (TMSOTf), so that the tedious operation of firstly protecting the hydroxyl group and then carrying out substitution reaction in the traditional method is avoided, and a key intermediate (d) required for preparing the anti-influenza virus derivative can be obtained in one step. The method has the advantages of simplicity and convenience in operation, high yield, easiness in industrial amplification and the like, and is suitable for large-scale preparation of the anti-influenza virus medicine and pharmaceutically acceptable salts, esters or solvates thereof.

This invention provides a naphthopyrimidine-fused-acid sugar derivative, its synthesis method, and its application, belonging to the field of pharmaceutical technology. The naphthopyrimidine-fused-acid sugar derivative has the structures shown in formulas (I) to (IV). These compounds are obtained by one-step cyclization via a condensation reaction with 1,8-diaminonaphthalene in an organic solvent under the catalysis of a trifluoromethanesulfonate catalyst, using a propionyl-protected and p-toluenesulfonated sugar as the starting material. The preparation method is efficient and simple. The compounds of this invention exhibit good anti-proliferative activity against colon cancer tumor cells.