171 results about "Fluoroacetic acid" patented technology

The invention relates to the technical field of organic synthesis, and discloses a preparation method of bromo-pyrrole nitrile. The method comprises the following steps: (1) mixing p-chlorophenylglycine, acetonitrile, trifluoroacetic acid and a catalyst, then dropwise adding acyl chloride and carrying out acylation reaction, and after the reaction is completed, purging with an inert gas; (2) under the inert gas, mixing the mixture obtained in the step (1) with inorganic salt, then dropwise adding 2-chloroacrylonitrile, carrying out cyclization reaction, and separating a liquid phase from the obtained mixture; and (3) under the inert gas, mixing the liquid phase obtained in the step (2), hydrobromic acid and hydrogen peroxide, carrying out a bromination reaction, then extracting with acetonitrile to obtain an acetonitrile layer, then removing the acetonitrile, and then carrying out cooling crystallization to obtain the bromo-pyrrolenitrile. According to the technical scheme, the reaction yield is high, different solvents do not need to be frequently replaced, and the solvents can be recycled.

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.

A method for producing an aromatic heterocycle-substituted difluoroacetic acid derivative having a partial structure represented by the formula (III), by reacting an N-oxido aromatic heterocyclic compound having a partial structure represented by the formula (I) with tetrafluoroethylene in the presence of a compound represented by the formula (II): R—YH, in a solvent selected from an aromatic hydrocarbon solvent, an ester solvent and an ether solvent:

The invention relates to a lithium ion battery. In order to solve the problem that the performance of the battery is influenced by solvent decomposition and gas production due to the fact that active oxygen is released in the using process when a lithium supplementing agent is added, a solvent ethylene carbonate in an electrolyte is promoted to be subjected to a ring-opening reaction, and the lithium ion battery comprises a positive electrode, a negative electrode, a diaphragm and the electrolyte, the positive electrode comprises a positive electrode active material and a lithium supplement agent, the electrolyte comprises an organic solvent, a lithium salt and an additive, the organic solvent comprises fluoro carboxylic ester, fluoro ether and carbonic ester and does not contain ethylene carbonate, and the additive comprises trimethylsiloxyethyl isocyanate and / or 2-(1, 1-thiophane-3-dioxide)-2, 2-methyl difluoroacetate. Through the synergistic effect of the solvent system and the additive, the stability of the electrolyte in a battery containing a lithium supplement agent is improved, the wettability and low-temperature performance of the battery, especially a high-compaction battery, are improved, and meanwhile, the lithium ion battery has relatively good normal-temperature cycle performance and high-temperature performance.

The invention belongs to the technical field of chromatographic separation materials, and discloses a preparation method and application of a GM-8 nanosheet material. The preparation method of the material comprises the following steps: respectively dissolving Cu (NO3) 2.3 H2O and 1, 3, 6, 8-tetra (4-carboxybenzene) pyrene in an organic solvent, mixing, transferring into a reaction bottle, adding trifluoroacetic acid and pyridine, and uniformly mixing and stirring to obtain a reaction mixture; and heating the reaction mixture to react for 7-9 hours to obtain a blue precipitate, cooling the blue precipitate to room temperature, and washing and drying the blue precipitate to obtain the ultra-stable microporous GM-8 nanosheet material. The nanosheet GM-8 is used as a gas chromatography stationary phase, high-efficiency separation and trace detection of xylene isomers can be realized, and the chromatographic column still keeps excellent separation capacity after being stored in an environment with air humidity of 65-90% for 31 months. The capillary gas chromatographic column can realize high-efficiency separation of disubstituted benzene isomers such as xylene, the separation degree of m-xylene / p-xylene is up to 18.2, and a new solution is provided for high-efficiency separation of isomers with similar properties.

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.

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 invention discloses an LC-MS (liquid chromatography-mass spectrometry) detection method for N, N-diethyl-N ', N'-dimethylethylenediamine in chlorpheniramine maleate, and belongs to the technical field of analytical chemistry. The method comprises the following steps: firstly, preparing a test solution and a reference solution for later use; then setting liquid chromatography-mass spectrometry detection conditions, and detecting N, N-diethyl-N ', N'-dimethylethylenediamine in chlorpheniramine maleate by adopting a Shim-pack Scept Diol-HILIC-120 chromatographic column, taking a 0.1% difluoroacetic acid aqueous solution-acetonitrile mixed solution as a mobile phase and taking a 1% diethylamine acetonitrile solution as a solvent. According to the method, a liquid chromatography-mass spectrometry technology is adopted, the problem that N, N-diethyl-N ', N'-dimethyl ethylenediamine has no ultraviolet absorption can be effectively solved, and meanwhile, the method is high in specificity, high in sensitivity and high in efficiency.

The application relates to the technical field of metal organic thin layer material preparation, in particular to a kilogram-level preparation method of metal organic thin layer material. The preparation method comprises the following steps: S1, adding zirconium tetrachloride and H2BPYDC into a polytetrafluoroethylene reaction kettle, dissolving the zirconium tetrachloride and the H2BPYDC, and then adding a composite; S2, sequentially adding a DMF solution of palladium fluoroacetate, a catalyst and concentrated hydrochloric acid into the reaction kettle; S3, transferring the reaction kettle into an oven, centrifuging to obtain a cyan suspension after 18-20 hours, dispersing the cyan suspension in a DMF solution in batches at 60 DEG C, placing for 5-6 hours, removing unreacted substrates, and obtaining a solid; S4, cleaning the solid obtained in S3 by using DMF and tetrahydrofuran respectively, and vacuum drying for 12 hours to obtain the metal organic thin layer material. The kilogram-level preparation method of metal organic thin layer material is provided, so as to solve the problems of low preparation yield, slow rate and difficulty in kilogram-level preparation of metal organic thin layer material in the related art.

The invention discloses a preparation method and application of a silicon-based functionalized fluorenyl polysubstituted acetylene copolymer and a gas separation membrane thereof. Belongs to the technical field of polymer material and gas separation. The invention provides a new thought for preparation of a high-permeability gas separation membrane material. The preparation method comprises the following steps: carrying out copolymerization on 1-phenyl-2-(7-trimethylsilyl-9, 9-bis (trimethylsilyl-fluorene-2-yl) acetylene and 1-phenyl-2-(7-trimethylsilyl-9, 9-dimethyl-fluorene-2-yl) acetylene under the catalysis of TaCl5-n-Bu4Sn, so as to prepare a copolymer with high molecular weight; the preparation method comprises the following steps of: carrying out film casting on a solution of the nano-silver oxide, and then carrying out desiliconization treatment by using normal hexane / trifluoroacetic acid to obtain a gas separation membrane with the thickness of 100-220 microns, the specific surface area of 298-492 m / g and the total pore volume of 0.134-0.299 cm / g. The prepared separation membrane has the advantages that the COpermeability is up to 36,900 Barrer, the Opermeability is 19,800 Barrer, the thermal decomposition temperature exceeds 420 DEG C, the separation membrane can be used for separating gases such as COO, ON and the like, the preparation process is simple and convenient, and the industrial potential is realized.

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 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 relates to a preparation method of trifluoromethylsulfonyl fluoride, which comprises the following steps: taking fluorosulfonyl difluoroacetic acid, fluorosulfonyl difluoroacetate or fluorosulfonyl difluoroacetyl fluoride as raw materials, and reacting with fluorine gas to obtain the product trifluoromethylsulfonyl fluoride. According to the method, the fluorosulfonyl difluoroacetic acid (ester or acyl fluoride) directly reacts with the fluorine gas, and complex multi-step reaction and separation and purification of intermediate products are not needed, so that the process flow is simplified, the production links are reduced, and the production efficiency is improved; the method has the advantages of low price of raw materials, mild reaction conditions, low requirements on equipment, realization of continuous production, and reduction of the equipment investment and the production cost; the preparation method is carried out under an anhydrous condition, does not need to use any organic solvent, and is environment-friendly and green; by controlling the reaction conditions, the yield of the trifluoromethylsulfonyl fluoride can reach 85%, the purity of the trifluoromethylsulfonyl fluoride can reach 99.9%, the requirements of different fields for high-purity products can be met, and the method has a good industrial application prospect.

The invention discloses bio-based polyamide with low water absorption and a preparation method thereof, and belongs to the technical field of polyamide preparation. The bio-based polyamide with the low water absorption rate is prepared from the following components in parts by weight: 30 to 50 parts of pentamethylene diamine, 15 to 30 parts of sebacic acid, 5 to 12 parts of citric acid, 5 to 10 parts of hexamethylenediamine, 2 to 5 parts of a hydrophobic auxiliary agent and 1 to 5 parts of a modified high-temperature-resistant additive, the hydrophobic additive is prepared from acetoxybenzoic acid, nonadecanoic acid, m-dimethoxybenzene, trifluoroacetic anhydride and methyl tert-butyl ether as raw materials, and the modified high-temperature-resistant additive is prepared from o-phenylenediamine, chloroacetic acid, vanillin, benzoyl bromide and thiourea as raw materials. The bio-based polyamide prepared from the substances has low water absorption and excellent thermal stability.

The invention discloses a method for microwave digestion of an express packaging material and application, and the method comprises the following steps: S1, crushing and grinding the express packaging material until the particle size is less than 100 [mu] m; s2, adding a composite acid-chitinase mixed solution into the digestion tank, and preliminarily contacting with the sample to weaken the structure of the sample; the composite acid-chitinase mixed solution comprises a composite acid mixed solution and a chitinase aqueous solution; the composite acid mixed solution comprises nitric acid, trifluoroacetic acid, hydrogen peroxide and formic acid; s3, placing the digestion tank treated in the step S2 on a turntable of a microwave digestion instrument, and carrying out pulse type microwave digestion; the microwave time is 25 minutes to 35 minutes; according to the method, pulse type microwaves are matched with the composite acid to digest the express packaging material, the digestion solution with high digestion completeness is obtained, HP-beta-CD and DTPA are used as double ligands to synergistically extract heavy metals such as lead and cadmium, the selectivity is good, and the efficiency is high.

The embodiment of the invention provides a bromo-ethyl difluoroacetate-mediated novel amide dehydration cyaniding method, which comprises the following steps of: heating and reacting 0.2 mmol and 1.0 equivalent weight of amide compound and 0.6 mmol and 3.0 equivalent weight of bromo-ethyl difluoroacetate for 24 hours under an oil bath condition of 90 DEG C to generate an experimental reactant; concentrating the experimental reactant under reduced pressure to obtain a residue; and purifying the residue by silica gel rapid column chromatography to obtain the target product nitrile compound. According to the scheme, the process reaction conditions are mild, a strict anhydrous and anaerobic environment is not needed, the harsh requirements on equipment and operation are greatly reduced, and the production safety and practicability are improved. Acetone is used as a solvent, so that high-efficiency reaction can be realized, the solvent after reaction is convenient to recycle and recycle, the production cost and the environmental burden are remarkably reduced, and the remarkable green chemical engineering characteristic is embodied.

The invention belongs to the technical field of electrolysis, and discloses a method for preparing p-hydroxyanisole through electrolytic oxidation of anisole. The method comprises the following steps: S1, adding anisole, an acylation reagent, an organic alkali proton trapping agent and an alkaline amine group-containing solvent into a single-chamber electrolytic bath together, starting electrification, carrying out electrolysis, and obtaining a product liquid containing p-methoxytrifluoroacetic acid phenyl ester in the single-chamber electrolytic bath after electrolysis is finished; the organic base proton trapping agent is at least one of N, N-diisopropylethylamine, tributylamine and tripropylamine; and S2, adding a saturated sodium bicarbonate aqueous solution into the product liquid containing p-methoxytrifluoroacetic acid phenyl ester in the step S1 to hydrolyze p-methoxytrifluoroacetic acid phenyl ester, and extracting to obtain p-hydroxyanisole. The selectivity of para-position and ortho-position products of methoxyl on anisole is regulated and controlled, so that the selectivity of p-hydroxyanisole prepared by the method is higher.

This invention belongs to the field of responsive material production technology, specifically relating to a high-viscosity fluoropolymer solution and its applications. The preparation method of the high-viscosity fluoropolymer solution is as follows: (meth)acrylate naphthyl ester, fluorinated methacrylate, and vinylcarbazole are dissolved in a solvent and stirred to obtain a clear and transparent solution. Then, an initiator is added, and the mixture is heated to 60-90℃ under magnetic stirring for 16-24 hours to polymerize. After the reaction is completed, a transparent high-viscosity polymer solution with a viscosity range of 800-8000 Pa·s is obtained. After the high-viscosity fluoropolymer solution forms a film on the substrate, it forms an anti-counterfeiting coating that can be stimulated by ultraviolet light and trifluoroacetic acid, exhibiting excellent multi-stimulus responsiveness. The preparation method of this anti-counterfeiting coating is simple, has good film-forming properties, long service life, and low cost. It can be industrially produced and provides dual anti-counterfeiting capabilities, showing great application prospects in anti-counterfeiting, information encryption, and other fields.

The application relates to the field of biological medicine, and discloses an active oxygen response thione aldehyde linker as well as a preparation method and application thereof. The thione aldehyde linker structure is a thione aldehyde structure with a p-hydroxyphenyl as a center. The thione aldehyde carbon atom is connected with two -CH2CH2COOH groups through a sulfur atom. The preparation method of the active oxygen response thione aldehyde linker comprises the following steps: dissolving 3-mercapto propionic acid and p-hydroxybenzaldehyde in ethyl acetate, adding trifluoroacetic acid as a catalyst, stirring and reacting at room temperature, and after the reaction is completed, the thione aldehyde linker is obtained through separation and purification. The thione aldehyde linker can respond to the increased ROS level in a tumor microenvironment, is broken under a high ROS condition, and thus realizes the release of a drug molecule connected therewith, which is beneficial to realizing the specific release of the drug at a tumor site.

The invention relates to the field of macromolecules, and discloses a method for refining polyetherketoneketone and a polyetherketoneketone refined product. The method comprises the following steps: (1) treating a polyetherketoneketone complex by adopting a pretreatment agent; (2) the polyether ketone ketone crude product and a mixed chain supporting solution are mixed and washed, a first product is obtained, the mixed chain supporting solution comprises a main chain supporting agent and a cosolvent, the main chain supporting agent comprises one or more selected from parachlorophenol, trifluoroacetic acid, difluoroacetic acid, dichloroacetic acid and chloroacetic acid, the cosolvent comprises one or more selected from N, N-dimethylformamide and dimethyl sulfoxide, and the main chain supporting agent comprises one or more selected from dichlorophenol, trifluoroacetic acid, difluoroacetic acid, dichloroacetic acid and chloroacetic acid. The solvent is one or more of water, N-methyl pyrrolidone and N-methyl formamide; (3) adding a mixed aqueous solution into the first product to remove at least part of metal ions to obtain a second product; and (4) washing the second product for multiple times by using an organic solvent, and washing and drying to obtain the refined polyether ketone ketone. The content of aluminum ions in the polyetherketoneketone prepared by the method is low.

The present invention relates to a 13 C. 18 The synthesis method of trifluoroacetic acid with O stable isotope double labeling is as follows: firstly, trifluoroacetic acid is dissolved in a solvent, metal ions are added, and 13 C-labeled carbon dioxide, react to obtain a reaction solution, then separate and dry the reaction solution to obtain 13 C-enriched trifluoroacetic acid, and finally 13 C-enriched trifluoroacetic acid is dissolved in an aprotic solvent, thionyl chloride is added, stirred for reaction, and then a catalyst and oxygen 18 water are added, heated for reaction, and the reaction product is separated to obtain 13 C. 18 O stable isotope double labeled trifluoroacetic acid is the target product. Compared with the prior art, the present invention has a simple reaction process, a simple post-processing process, and a high yield. 13 The C isotope abundance is over 98%. 18 The O isotope abundance is over 97%.

The application relates to the field of liquid chromatography analysis, and provides a method for high-performance liquid chromatography analysis of DNA dyes, which comprises the following steps: performing high-performance liquid chromatography analysis on a DNA dye-containing sample to be measured; wherein the DNA dye comprises at least one of PicoGreen and SYBR Green I; the high-performance liquid chromatography analysis adopts gradient elution, and mobile phase A, mobile phase B and mobile phase C are mixed in different proportions as mobile phases; the mobile phase A comprises at least one of acetonitrile and methanol; the mobile phase B comprises at least one of phosphoric acid aqueous solution, formic acid aqueous solution and trifluoroacetic acid aqueous solution; and the mobile phase C comprises ammonium acetate aqueous solution. The method can be used for detecting the purity of Picogreen, SYBR Green I and the DNA dyes, and realizes effective separation of target peaks and impurity peaks.

This invention belongs to the field of biochemistry technology, and relates to a near-infrared chemiluminescent probe responsive to tau protein, its preparation method, and its application. The preparation method of the near-infrared chemiluminescent probe includes the following steps: adding compound (I), compound (II), a catalyst, and an alkaline additive to a first solvent for reaction to obtain compound (III); adding compound (III), compound (IV), and piperidine to a second solvent for reaction to obtain compound (V); adding compound (V) and trifluoroacetic acid to a third solvent for reaction to obtain compound (VI); and adding compound (VI), compound (VII), and an acid compound to a fourth solvent for reaction to obtain the near-infrared chemiluminescent probe. The chemiluminescent probe of this invention exhibits high selectivity and efficient chemiluminescence capability, providing a promising tool for the diagnosis of Alzheimer's disease (AD). Its structural formula is: [Insert structural formula here].

The present invention belongs to the field of medicinal chemistry and relates to a triazine-thiazolidinone compound and its preparation method and application. Its structural formula is wherein R1 is any one of alkyl, pyranyl, indolyl, phenyl or thienyl. Its pharmaceutically acceptable salt is the acid salt of the compound, and the acid is any one of hydrochloric acid, hydrobromic acid, sulfuric acid, phosphoric acid, boric acid, methanesulfonic acid, p-toluenesulfonic acid, naphthalenesulfonic acid, benzenesulfonic acid, citric acid, lactic acid, pyruvic acid, tartaric acid, acetic acid, trifluoroacetic acid, maleic acid, succinic acid, mandelic acid, fumaric acid, salicylic acid or phenylacetic acid. The triazine-thiazolidinone compound skeleton provided by the present invention is novel, has a good inhibitory effect on glucose transporter 1 (GLUT1), and its inhibitory effect in HT29 cells is much better than that of positive control compound BAY-876, with good potential for further development as an anti-tumor drug.

The application relates to the technical field of compound synthesis, and discloses an aromatic dipeptide functionalized mercapto compound, 3,5-di(triphenylmethylthio)benzoic acid is obtained by adding 3,5-di(methylmercapto)benzoic acid and pyridine into a solution of chloromethyl triphenylphosphonium, purifying after sufficient reaction; then the 3,5-di(triphenylmethylthio)benzoic acid is mixed with N-hydroxysuccinimide and dissolved in an organic solvent, EDC.HCl is added, purifying after sufficient reaction; then 2,5-dioxopyrrolidin-1-yl 3,5-bis(triphenylmethylthiomethyl)benzoate is obtained; then phenylalanine-tryptophan and triethylamine are added, purifying after sufficient reaction; then (3,5-bis(triphenylmethylthiomethyl)benzoyl)tryptophylphenylalanine is obtained; then trifluoroacetic acid and triethylsilane are added, purifying after sufficient reaction; and finally the aromatic dipeptide functionalized mercapto compound is obtained. The aromatic dipeptide functionalized mercapto compound can quickly and effectively identify sodium and potassium ions, and has relatively low detection limit and relatively loose detection condition.

The invention discloses an HPLC (High Performance Liquid Chromatography) detection method for ipragmine hydrochloride enantiomers, and belongs to the technical field of pharmaceutical analysis. The HPLC detection method provided by the invention comprises the following steps: dissolving ipragmine hydrochloride to be detected in a diluent to prepare a test solution; detecting the test solution by adopting normal-phase high performance liquid chromatography; the stationary phase of the normal-phase high performance liquid chromatography is silica gel of which the surface is covalently bonded with cellulose-tri (3-chloro-4-methyl phenyl carbamate); a mobile phase of the normal-phase high performance liquid chromatography is a mixed solution of normal hexane, isopropanol, trifluoroacetic acid and diethylamine. According to the detection method established by the invention, the ipragmine hydrochloride main peak and the S-configuration enantiomer impurity peak can be subjected to baseline separation, the separation degree can reach 4.5 or above, the method is high in specificity and sensitivity, and various methodology verification parameters all meet the drug quality control requirements.

The present invention relates to the technical field of pharmaceutical chemistry, and to a method for synthesizing a doravirine intermediate. The synthesis method of the present invention comprises: (1) mixing ethyl 2-fluoroacetate with 4-ethoxy-1,1,1-trifluoro-3-buten-2-one in a first solvent and adding sodium bis(trimethylsilyl)amide for a reaction to generate compound 1; (2) adding triethylamine and trifluoroacetic anhydride to a reaction solution of compound 1 for a reaction to generate compound 2; (3) adding an ammonia source to a reaction solution of compound 2 to obtain compound 3 and compound 4; and (4) adding a second solvent and heating the resulting mixture for cyclization to obtain 2-hydroxy-3-fluoro-4-trifluoromethylpyridine. The present invention has low raw material cost and is a synthesis method, which has a short process cycle, is environmentally friendly, and is suitable for scale-up process production.

The invention belongs to the technical field of biochemistry, and relates to a ratio type probe compound, a preparation method thereof, a Cu (I) response photoacoustic probe composition and application. The preparation method of the ratiometric probe compound comprises the following steps: (1) reacting a compound (I), a compound (II), acetic acid and piperidine to obtain a compound (III); (2) reacting the compound (III) with trifluoroacetic acid to obtain a compound (IV); (3) carrying out a reaction on the compound (IV), the compound (V), 2-(7-azabenzotriazole)-N, N, N ', N'-tetramethylurea hexafluorophosphate and 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride, so as to obtain a compound (VI); and (4) reacting the compound (VI), the compound (VII), acetic acid and piperidine to obtain the compound. The photoacoustic probe provided by the invention has excellent selectivity and high sensitivity.

This invention discloses an acylhydrazone-linked covalent organic framework material, its preparation method, and its application, belonging to the field of covalent organic framework material synthesis technology. The preparation method of the acylhydrazone-linked covalent organic framework material is as follows: benzo[1,2-b:3,4-b':5,6-b”]trithiophene-2,5,8-tricarboxaldehyde, benzodiazepine, o-dichlorobenzene, and n-butanol are mixed to obtain suspension A; trifluoroacetic acid is added to suspension A and mixed to obtain mixture A; mixture A is sequentially subjected to freeze degassing and heating treatment, followed by extraction to obtain the final product. This invention uses benzo[1,2-b:3,4-b':5,6-b”]trithiophene-2,5,8-tricarboxaldehyde and benzodiazepine with a specific structure as main raw materials, and by adjusting the concentration, type, and amount of catalyst, an acylhydrazone-linked covalent organic framework material with higher crystallinity and stability is prepared.