440 results about "Trifluoroacetic acid" patented technology

Development of resists are useful, for example, to form a patterning mask in the context of high-resolution patterning. Development can be accomplished using an organic vapor such as a carboxylic acid. In some implementations, the organic vapor is trifluoroacetic acid. In some implementations, the organic vapor is hexafluoro-acetylacetone. A metal-containing resist film such as an EUV-sensitive organo-metal oxide may be deposited on a semiconductor substrate using a dry or wet deposition technique. The metal-containing resist film on the semiconductor substrate may be developed using the organic vapor, or residue of metal-containing resist material formed on surfaces of a process chamber may be removed using the organic vapor.

The invention relates to the technical field of chemical synthesis, and particularly provides a preparation method of a semaglutide side chain, which comprises the following steps: step S1, carrying out reaction on octadecanedioic acid mono-tert-butyl ester and trifluoroacetic acid pentafluorophenyl ester to generate a first intermediate; s2, enabling the first intermediate to react with 1-tert-butyl L-glutamic acid to generate a second intermediate; s3, enabling the second intermediate to react with pentafluorophenyl trifluoroacetate to generate a third intermediate; and S4, carrying out an amidation reaction on the third intermediate and 17-amino-10-oxo-3, 6, 12, 15-tetraoxa-9-aza-heptadecanoic acid, so as to generate a semaglutide side chain, and carrying out an amidation reaction on the third intermediate and 17-amino-10-oxo-3, 6, 12, 15-tetraoxa-9-aza-heptadecanoic acid. According to the preparation method disclosed by the embodiment of the invention, the pentafluorophenyl trifluoroacetate is used as the condensation reagent for two times to activate the carboxylic acid, and the amidation reaction is carried out for two times to construct the amido bond after each activation, so that compared with the traditional carbodiimide and urea positive ion type condensation reagent, the chiral racemization in the condensation process can be effectively avoided, and the yield of the product is improved. The condensation chiral racemization impurity can be lower than 0.3%.

The invention discloses a covalent organic framework membrane and a preparation method thereof, and belongs to the technical field of organic porous materials and membrane materials. The preparation method of the covalent organic framework membrane comprises the following steps: S1, respectively dissolving an amine compound containing a plurality of amino groups and a compound containing a plurality of aldehyde groups in a mixed solution of trifluoroacetic acid and water to respectively obtain a first monomer solution and a second monomer solution; in the mixed solution, the volume ratio of trifluoroacetic acid to water is (95-96): (4-5); s2, mixing the first monomer solution and the second monomer solution, and performing ultrasonic treatment to obtain a reaction solution; and heating the reaction liquid at 95-100 DEG C to react for 3-5 minutes to form the covalent organic framework film. In addition, the invention also provides the covalent organic framework film which is prepared by the preparation method. The COF film which is complete in structure, excellent in crystallinity and flexible can be prepared in a short time through a simple method.

The invention provides a content detection method for a salvia miltiorrhiza medicinal material, a salvia miltiorrhiza clear paste and a musk heart-dredging dropping pill. According to the method, a high performance liquid chromatography method is adopted, octadecylsilane chemically bonded silica is used as a chromatographic column filler, acetonitrile is used as a mobile phase A, 0.02%-0.1% trifluoroacetic acid is used as a mobile phase B, gradient elution is carried out, and rosmarinic acid and salvianolic acid B in the salvia miltiorrhiza medicinal material are synchronously and quantitatively detected. And synchronously and quantitatively detecting tanshinol, protocatechuic aldehyde, caffeic acid, salvianolic acid E, rosmarinic acid, alkannic acid and salvianolic acid B in the salvia miltiorrhiza clear paste, and synchronously and quantitatively detecting tanshinol, protocatechuic aldehyde, caffeic acid, salvianolic acid E, rosmarinic acid, alkannic acid, salvianolic acid B, arenobufagin and bufalin in the musk Tongxin dropping pill. The method is used for monitoring the content of specific components, can also judge the transfer rate in the medicine production process, and facilitates traceability in the production link. In addition, the method is relatively low in equipment requirement and suitable for industrial popularization.

The invention provides an anion exchange polymer and a preparation method thereof and an anion exchange membrane, the anion exchange polymer comprises a chain segment I and / or a chain segment II, the structural formula of the chain segment I is # imgabs0 #, the structural formula of the chain segment II is # imgabs1 #, A is nitrogen-containing heterocyclic ketone, Ar1 is a first aryl structural unit, Ar2 is a second aryl structural unit, and the structural formula of the chain segment II is # imgabs1 #. M <-> is a trifluoroacetic acid ion and / or a p-toluenesulfonate ion. The anion exchange polymer disclosed by the invention is relatively low in toxicity to a catalyst, so that the anion exchange polymer shows excellent electrochemical performance.

The invention provides a method for detecting diastereoisomers in a nerofloxacin malate sodium chloride injection. The method comprises the following steps: separating optical isomers of the nerofloxacin malate sodium chloride injection by adopting a liquid chromatography; wherein the chromatographic condition of the liquid chromatography comprises a mobile phase, the mobile phase comprises a mobile phase A and a mobile phase B, the mobile phase A is a trifluoroacetic acid solution, and the mobile phase B is methanol-tetrahydrofuran. According to the technical scheme, a trifluoroacetic acid solution is adopted as a mobile phase A, methanol-tetrahydrofuran is adopted as a mobile phase B, tetrahydrofuran is added in the mobile phase B, the peak pattern of a main peak is improved, the trailing factor is 1.06, the operation time can be shortened, and the peak pattern of the main peak is improved.

The invention relates to an anti-hair loss and hair growth peptide with alternately arranged D / L amino acids as well as a preparation method and application of the anti-hair loss and hair growth peptide, and belongs to the technical field of biological medicines. The amino acid sequence of the polypeptide is shown as SEQ ID NO: 1, D-type and L-type amino acids are alternately arranged and designed, the protease degradation resistance is remarkably enhanced, the in-vitro half-life period is larger than or equal to 48 hours, and beta-catenin protein expression in hair follicle stem cells is activated. The preparation method comprises the following steps: taking Rink Amide resin as a carrier, sequentially coupling D / L type amino acid by adopting an Fmoc solid-phase synthesis method, cracking the resin by trifluoroacetic acid, and purifying by high performance liquid chromatography, so that the yield is more than or equal to 80%, the purity is more than or equal to 96%, and the molecular weight is confirmed to be 956.12 Da by mass spectrometry. The polypeptide can be applied to preparation of anti-hair loss and hair growth cosmetics, medicines and medical instruments, and effectively solves the problems of low stability and insufficient targeting of the polypeptide in the prior art. # imgabs0 #

The invention provides synthesis and oxygen reduction application of a metal cluster / polyphthalocyanine network compounded organic electrocatalytic material. The preparation method comprises the following steps: by taking benzene ring-containing anhydride, chlorate and urea as raw materials, carrying out high-temperature reaction, cooling, and purifying for multiple times, so as to obtain an edge-functionalized polyphthalocyanine network precursor; dispersing the obtained polyphthalocyanine network precursor into a solution A by using a proper solvent; meanwhile, trifluoroacetate and a tert-butyl metal compound are mixed in a proper solvent to form a metal cluster, and the metal cluster compound is dissolved in the solvent to form a solution B; and mixing the two solutions, standing overnight, filtering, purifying, and carrying out ball milling treatment to finally obtain the target metal cluster / polyphthalocyanine network composite organic catalyst. The polyphthalocyanine oxygen reduction organic catalytic material designed by the invention is low in raw material cost and simple to prepare. The test shows that the half-wave potential of the material is 100 mV higher than that of Pt / C, the E1 / 2 reduction value is 30 mV lower than that of Pt / C after accelerated aging for 2500 circles, and the material has high activity and high stability and can be applied to devices such as lithium batteries and fuel batteries related to the oxygen reduction process.

The invention provides a sulfonated modified COF-based hydrogel based on a TPAD skeleton, and a preparation method and application thereof, and belongs to the field of water treatment. The preparation method comprises the following steps: S1, synthesizing a TPAD-NHBoc amino monomer by using reagents such as 1, 4, 5, 8-tetrachloroanthraquinone and the like; s2, sequentially adding a TPAD-NHBoc amino monomer, a Dha aldehyde monomer, dioxane and trifluoroacetic acid into a glass tube according to a certain proportion, carrying out ultrasonic treatment, stirring, putting into a reaction kettle, and reacting at 115-125 DEG C for 96-120 hours; s3, after the reaction is finished and cooling is performed, carefully taking out the blocky gel from the glass tube, respectively immersing the blocky gel into dioxane and DMF, and repeatedly replacing the solvent for washing; s4, washing the gel, soaking the washed gel in a DMF solution containing 1, 3-propane sultone, and carrying out a reaction at 75-85 DEG C for 16-20 h to obtain sulfonated modified gel; s5, the obtained sulfonated modified COF-based gel is soaked in DMF, acetone, methanol and water for multiple times of soaking and washing, and the hydrogel is obtained. The sulfonated modified hydrogel based on the TPAD skeleton has excellent solar photo-thermal water evaporation performance.

The invention relates to the technical field of photo-thermal therapy, in particular to a monomolecular photo-thermal agent with high photo-thermal conversion efficiency and a preparation method and application of the monomolecular photo-thermal agent. The preparation method comprises the following steps: S1, synthesis of a compound X1: under the protection of argon, dissolving 2, 4-dimethyl pyrrole in dichloromethane, stirring in an ice bath, adding trifluoroacetic anhydride, heating to room temperature after stirring, extracting after quenching reaction, combining organic phases, drying, filtering, concentrating under reduced pressure and purifying by silica gel column chromatography to obtain the compound X1. The prepared monomolecular photothermal agent with the high photothermal conversion efficiency is high in water solubility, has the high photothermal conversion efficiency in an aqueous solution and is high in light stability, the immune escape phenomenon possibly caused by introduction of a high polymer material is avoided, and the technical problem that an existing photothermal agent is difficult to achieve the high photothermal conversion efficiency in the aqueous solution is solved.

The invention relates to the technical field of compound preparation, and particularly provides a preparation method of alkyl cyclophosphoric anhydride, which comprises the following step: reacting alkyl phosphoric acid with trifluoroacetic anhydride to generate alkyl cyclophosphoric anhydride. The preparation method provided by the embodiment of the invention has the advantages of simple operation, high reaction activity, low reaction temperature, short reaction time and easy raw material recovery, and is suitable for industrial production. Besides, the boiling point difference between the residual raw material trifluoroacetic anhydride and the by-product trifluoroacetic acid reaches 32 DEG C, the trifluoroacetic anhydride can be well separated through rectification, and the separated and recycled trifluoroacetic anhydride can be further used for reaction, so that the production cost is greatly reduced.

The invention discloses a synthesis method of 2, 4, 5-trifluorophenylacetic acid, which comprises the following steps: by taking cheap and easily available o-chloronitrobenzene as a raw material, reacting with sodium nitrate in a sulfuric acid and trifluoroacetic acid system, separating generated 2, 4-dinitrochlorobenzene through melt crystallization, and continuing to synthesize 2, 4-dinitrochlorobenzene in methyl chloroacetate to obtain 2, 4, 5-trifluorophenylacetic acid. The method comprises the following steps: carrying out indirect aromatic nucleophilic substitution reaction on 2, 4-dinitrophenylacetic acid under the condition of sodium hydride to generate 5-chloro-2, 4-dinitrophenylacetic acid methyl ester, separating, carrying out fluorination reaction on the 5-chloro-2, 4-dinitrophenylacetic acid methyl ester and potassium fluoride under the action of a phase transfer catalyst, carrying out rectification separation to obtain 2, 4, 5-trifluorophenylacetic acid, and carrying out hydrolytic acidification on the 2, 4, 5-trifluorophenylacetic acid in a sodium hydroxide aqueous solution to obtain 2, 4, 5-trifluorophenylacetic acid. And the process route is safer, more environment-friendly, more efficient and lower in cost.

The invention relates to the field of skin care products, and discloses a ceramide liposome for skin care products and a preparation method thereof, the ceramide liposome comprises the following components by weight: 5-10 parts of hydrogenated lecithin, 0.5-2 parts of modified cholesterol, 0.5-2 parts of ceramide, 0.1-2.5 parts of sucrose stearate, 0.1-1 part of polyglycerol-10 stearate, and 15-30 parts of an organic solvent; the modified cholesterol is prepared by grafting glycine cholesteryl ester and carboxymethyl chitosan through a chemical reaction, the glycine cholesteryl ester is prepared from cholesterol, N-t-butyloxycarboryl glycine and trifluoroacetic acid as raw materials, and the carboxymethyl chitosan is prepared by grafting chloroacetic acid and chitosan. According to the invention, hydrogenated lecithin, modified cholesterol, ceramide, sucrose stearate and polyglycerol-10 stearate are used as raw materials to prepare the ceramide liposome with good stability, good skin barrier repairing property and good moisturizing and water locking effects.

The invention discloses a method for improving the stability of a polypeptide containing multiple cysteines in solid-phase synthesis, and mainly solves the technical problem of poor stability of the polypeptide caused by easy oxidation, degradation, elimination, denaturation and inactivation of the polypeptide. Comprising the following steps: 1) purifying polypeptides containing multiple cysteines synthesized by a solid phase through liquid chromatography to obtain a preparation solution containing trifluoroacetate; 2) enabling the prepared liquid to pass through a deep filter filled with hydrophilic silicon dioxide aerogel balls as a filter material, and adsorbing and removing metal ions and trace peroxides contained in the prepared liquid; 3) treating the prepared solution with the weakly alkaline cation exchange resin, wherein the pH value is 6.3-6.5; the preparation method comprises the following steps of 1, preparing a sodium trifluoroacetate solution, 2, preparing the sodium trifluoroacetate solution, 4, removing sodium trifluoroacetate in the prepared solution by using a tangential flow filtration method and applying low-pressure driving to obtain a weakly acidic salt-free prepared solution, 5, carrying out freezing and vacuum drying to obtain a solid powder final product, 6, carrying out vacuum packaging and freeze storage, and 7, carrying out purity stability according with scientific research after storage.

The invention discloses preparation of a dual-functionalized ionic liquid modified boron nitride heat-conducting filler and application of the dual-functionalized ionic liquid modified boron nitride heat-conducting filler in a heat-conducting composite material, and belongs to the field of heat-conducting materials. A novel modified filler (f-IL (at) BNNS) is prepared by using a green, stable and pollution-free ionic liquid, namely sulfonyl functionalized imidazole trifluoroacetate (f-IL), through a mild and easy-to-operate reaction process, and the filler is tightly combined with a matrix to form a long-range ordered heat conduction path, so that the composite material has excellent heat conduction performance.

The invention belongs to the technical field of drug synthesis, and particularly discloses a preparation method of a low-single-impurity and high-purity olpinapone intermediate 05, which comprises the following steps: adding UHP into a dichloromethane solution of an intermediate 04 while cooling, and keeping stirring for 0.5-1 hour; adding trifluoroacetic anhydride at a controlled low temperature, returning the temperature after adding, and carrying out heat preservation and stirring reaction; after the reaction is finished, filtering, leaching a filter cake with dichloromethane, washing filtrate with water, adding a material subjected to vacuum concentration into methylbenzene, adding formic acid, heating and stirring, cooling after stirring, filtering, collecting a filter cake, and drying under reduced pressure to obtain the low-single-impurity and high-purity olpinapone intermediate 05.

To provide an electrolyte for a power storage device that can suppress oxidation corrosion of an electrode current collector and provide excellent battery characteristics.SOLUTION: An electrolyte for a power storage device including water or an organic solvent as a solvent contains a trifluoroacetate (TFA) salt. The TFA salt reacts with aluminum metal present within a secondary battery to form a passivation film, thereby providing suppression capability against oxidation corrosion of the aluminum metal. The aluminum metal constitutes the material forming a cathode current collector and / or an anode current collector in the power storage device.SELECTED DRAWING: Figure 1

The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to a detection method of an evocamide enantiomer, which comprises the following steps: S1, preparing a test solution; s2, preparing a contrast solution; s3, preparing a system applicable solution; s4, carrying out a system applicability test; s5, testing a test sample and a contrast solution; a chromatographic column is a chiral chromatographic column taking a polysaccharide derivative or a cellulose derivative as a filler, and a mixed solution of n-hexane, isopropanol, trifluoroacetic acid and diethylamine is taken as a mobile phase to detect the Evocadum enantiomer. The method has the characteristics of simplicity in operation, high sensitivity and high accuracy, the chromatographic peaks are high in separation degree, do not interfere with one another, the peak shape is good, the result accuracy is guaranteed, the method can be used for detecting enantiomers in the Evocamide and the Evocamide preparation, the level of the enantiomers of the Evocamide is effectively controlled, and the medication safety is guaranteed.

The present invention discloses a photocatalyst for the regeneration of coenzyme NADH and a preparation method thereof, wherein the photocatalyst is a donor-π-acceptor type conjugated organic polymer, with a triazine-based ligand as an acceptor unit and a heterocyclic ligand as a donor unit, wherein the molar ratio of the triazine-based ligand to the heterocyclic ligand is 1:(1-2), the triazine-based ligand raw material selects 2,4,6-trimethyl-1,3,5-triazine, and the heterocyclic ligand raw material selects a heterocyclic diformaldehyde containing a furan or thiophene structure. The photocatalyst is prepared by a solvothermal method through a Knoevenagel aldol condensation reaction, the reaction solvent selects a mixed solvent of n-butanol and o-dichlorobenzene or a mixed solvent of mesitylene and 1,4-dioxane, and the catalyst used in the reaction selects at least one of trifluoroacetic acid, potassium hydroxide, 1,8-diazabicycloundecane-7-ene, sodium hydroxide, and cesium carbonate. The developed photocatalyst has a donor-π-acceptor type conjugated structure, and has high catalytic activity, high selectivity, good stability, and easy separation and recovery for the regeneration of coenzyme NADH.

A high-entropy nano-array for electrocatalytic nitrate reduction coupling waste plastic conversion is prepared by the following method: (1) immerse the nickel foam into a hydrochloric acid solution to remove the surface oxide layer and oil stains, rinse with deionized water / ethanol three times, and dry for subsequent use; (2) solid powders of sodium chloropalladate, platinum acetylacetate, nickel chloride hexahydrate, copper chloride dihydrate, silver trifluoroacetate and tungsten hexacarbonyl are poured into an N-N dimethylformamide solution, ultrasonic is used to dissolve the solid powders, then glacial acetic acid and the treated nickel foam are added to the above solution, and after ultrasonic, heating in an oven is carried out, after the reaction is completed, water and ethanol solution are used for alternate washing, and drying is carried out, and the high-entropy nano-array catalyst is obtained. A preparation method of a high-entropy nano-array for electrocatalytic nitrate reduction coupling waste plastic conversion is provided. The high-entropy nano-array has excellent electrocatalytic activity and stability.

An object is to provide a method of producing a carboxylic acid fluoride at an increased product yield in a reaction system without forming HCl as a by-product, in other words, without forming a complex between HCl and a carboxylic acid fluoride as a product.The method comprising reacting a carboxylic acid chloride with a metal fluoride. In this production method, the carboxylic acid is a carboxylic acid having a carbon number of 1 to 7, the carboxylic acid is a carboxylic acid substituted with fluorine, or the carboxylic acid is trifluoroacetic acid.

The invention provides a synthetic method of a bromo-pyrazole intermediate for preparing loratinib, which comprises the following steps: 1, adding a solvent and a compound 19 into a reaction kettle, and then adding a bromination reagent N-bromo-succinimide in batches to synthesize a compound 14; 2, adding dichloromethane, the compound 14 and triethylamine into a reaction kettle, and then dropwise adding trifluoroacetic anhydride to synthesize a compound 15, namely the key intermediate bromo-pyrazole of the loratinib; according to the synthetic method of the bromo-pyrazole intermediate for preparing the loratinib, the adopted starting materials are low in price, the route is simple, the yield is high, the purity is good, the cost is reduced by 40% or above compared with an existing synthetic route, the production cost can be greatly reduced, and the industrial competitiveness is improved.

The application relates to the technical field of analytical chemistry, in particular to a high-performance liquid chromatography analysis method for maleic acid olmutant, wherein the mobile phase in the high-performance liquid chromatography condition comprises mobile phase A and mobile phase B, the mobile phase A is a mixed solution, the mixed solution comprises trifluoroacetic acid, triethylamine and water, the volume fraction of trifluoroacetic acid in the mixed solution is 0.08-0.12%, the volume fraction of triethylamine is 0-0.3%, the mobile phase B is acetonitrile, and the volume ratio of the mobile phase A and the mobile phase B is 75:25-85:15. The trifluoroacetic acid and the triethylamine in the mobile phase are matched, the interaction between maleic acid olmutant and a chromatographic column is hindered, the peak shape is symmetrical, and peak tailing is significantly improved; meanwhile, the two can also form a buffer system; in addition, the trifluoroacetic acid can enhance the retention capacity of maleic acid olmutant on the chromatographic column and improve separation selectivity.

The invention discloses a positive pole piece and a preparation method thereof, a diaphragm-free battery and a battery. The positive pole piece comprises a positive pole current collector and a positive pole active material layer arranged on at least one side of the positive pole current collector, the positive pole active material layer comprises a polymer, and the polymer is formed by polymerizing at least one of small molecules of the following raw material components: vinylethylene carbonate, vinylene carbonate, 2, 3, 4-trimethyl-1, 3-pentanedione, 2, 3, 4-trimethyl-1, 3-pentanedione and 2, 3, 4-trimethyl-1, 3-pentanedione. The adhesive is prepared from 2, 4-hexadienoic acid, allyl trifluoroacetate, diethyl allylmalonate, allyl methacrylate, allyl chloroformate, allyl phenylacetate, allyl acetate, allyl 4-hydroxybenzoate and allyl phenoxyacetate. The adhesive is prepared from the following raw materials: 1, 4-hexadienoic acid, allyl trifluoroacetate, diethyl allylmalonate, allyl methacrylate, allyl chloroformate, allyl phenylacetate, allyl acetate, allyl 4-hydroxybenzoate and allyl phenoxyacetate. The positive pole piece provided by the invention comprises the polymer, so that the interface impedance can be reduced, and the rate capability of the battery can be improved.

The present application relates to the field of analytical chemistry, and provide a kind of method for detecting complex matrix of agricultural products in guanidine morpholino salt hydrochloride.The extraction solvent of the present application uses acetonitrile+acid+aqueous solution, different acid is selected according to the water content of sample, trifluoroacetic acid is used for high water content sample, and formic acid is used for low water content sample;In purification, pH value is adjusted according to the oil content of sample, ammonia is used to adjust pH to 8.5 for high oil content sample, and pH value can not be adjusted for low oil content sample.In the method, NaCl is not added to make organic phase and aqueous phase in extraction liquid stratified, through the way of extracting three times repeatedly, the recovery rate of the method is guaranteed;And using ultra-high phase liquid chromatography triple quadrupole mass spectrometry technology, guanidine morpholino salt hydrochloride in complex matrix of agricultural products is successfully detected, the extraction method is fast and simple, the quantitative limit of guanidine morpholino salt hydrochloride in tea is 0.1mg / kg, and the quantitative limit in other matrix is 0.05mg / kg, which is suitable for routine analysis, and can meet the quantitative detection requirements of guanidine morpholino salt hydrochloride in complex matrix of agricultural products.

FIELD: pharmacology.SUBSTANCE invention can be used to determine the concentration of an anti-tuberculosis drug in blood serum. The method for determining the concentration of bedaquiline in the blood serum in patients with tuberculosis or mycobacteriosis is that whole blood samples are centrifuged at 3000 rpm for 20 minutes, then the blood plasma is collected in sterile 1.5 mL Eppendorf tubes, then 900 mcL of acetonitrile are added to 300 mcL of plasma and centrifuged at 13500g for 15 minutes, then 1 mL of the supernatant is transferred to a chromatographic vial and make the assay by UHPLC MS / MS using an Athena UHPLC C18, 1.8 mcM, 120A, 2.1×100 mm chromatography column, when using an aqueous solution containing 5 g / L of ammonium acetate, 25 ml / L of concentrated acetic acid, 2 ml / L trifluoroacetic acid as mobile phase A and 100% acetonitrile as mobile phase B, the concentration of bedaquiline is determined using a pre-plotted calibration curve.EFFECT: determination of bedaquiline in human blood plasma in a time not exceeding 6 minutes.1 cl, 9 dwg, 6 tbl

The invention relates to the technical field of analytical chemistry, in particular to a high performance liquid chromatography analysis method of olatinib maleate, a mobile phase in high performance liquid chromatography conditions comprises a mobile phase A and a mobile phase B, the mobile phase A is a mixed solution, the mixed solution comprises trifluoroacetic acid, triethylamine and water, and the mobile phase B is a mixed solution. The mobile phase A is a mixed solution, the volume fraction of trifluoroacetic acid in the mixed solution is 0.08-0.12%, the volume fraction of triethylamine in the mixed solution is 0-0.3%, the mobile phase B is acetonitrile, and the volume ratio of the mobile phase A to the mobile phase B is 75: 25-85: 15. According to the invention, through the cooperation of trifluoroacetic acid and triethylamine in a mobile phase, the interaction between the oxilatinib maleate and a chromatographic column is hindered, so that the peak shape is symmetrical, and the peak trailing is obviously improved; meanwhile, the two can form a buffer system; in addition, the trifluoroacetic acid can enhance the retention capacity of the olatinib maleate on the chromatographic column and improve the separation selectivity.

This invention discloses a method for preparing the DPP1 inhibitor bresocarte, belonging to the field of pharmaceutical synthesis. Specifically, the method includes the following steps: N-tert-butoxycarbonyl-L-4-bromophenylalanine reacts with methanesulfonyl chloride or 4-nitrobenzenesulfonyl chloride in the presence of a base, followed by amination substitution to obtain intermediate 1; then, it undergoes dehydration in the presence of trifluoroacetic anhydride to obtain intermediate 2; next, it undergoes a coupling reaction with pinacol diboronate to obtain intermediate 3; then, it undergoes a coupling reaction with bromide compound 4 to obtain intermediate 5; then, it undergoes cyclization with di-tert-butyl dicarbonate in the presence of sodium methoxide to obtain intermediate 6; then, it undergoes deprotection in the presence of hydrogen chloride to obtain intermediate 7; next, it undergoes condensation with compound 8 to obtain intermediate 9; finally, it undergoes deprotection in the presence of hydrogen chloride to obtain the inhibitor bresocarte. This method provides a new synthetic approach, with low overall cost, simple operation, high yield, and suitability for industrial production.

The invention provides a method for preparing 2, 6-diamino-3, 5-dinitropyridine, which comprises the following steps: (1) reacting 2, 6-diaminopyridine with an amino protection reagent to obtain an intermediate A; (2) in the presence of a dehydrating agent, carrying out double nitration reaction on the intermediate A and a nitration reagent to generate an intermediate B; (3) 2, 6-diamino-3, 5-dinitropyridine is obtained after the intermediate B is subjected to deprotection, and an amino protection reagent is selected from one or more of acetic anhydride, trifluoroacetic anhydride, di-tert-butyl dicarbonate, benzyl chloroformate and concentrated sulfuric acid; wherein the molar ratio of the amino protection reagent to the 2, 6-diaminopyridine is (2: 1)-(30: 1) by mole; and preferably, the ratio is 2: 1-12: 1.

The invention belongs to the technical field of electrolyzed water, and particularly relates to an electrolyte additive for improving the reaction performance of electrolyzed water, an electrolyte, an electrolyte solution and a method for improving the reaction performance of electrolyzed water. The additive comprises nonmetal oxosalts (sulfate, phosphate, borate, selenate, silicate, carbonate, perchlorate, trifluoroacetate and the like) and an aqueous solution of the nonmetal oxosalts, and is used as an electrolyte additive for water electrolysis reaction with KOH or NaOH as an electrolyte. The invention provides application of oxysalt to improvement of oxygen evolution activity and stability of electrolyzed water. In particular, the device is also suitable for electrolytic reactions carried out at high and low temperatures. Due to the addition of the oxysalt, the oxygen evolution reaction potential is reduced, the charge transfer resistance is reduced, the electron transmission rate is increased, and relatively high chemical reaction kinetics is achieved, so that the reaction activity is favorably improved.