237 results about "Fluoroacetic acid" patented technology

The invention relates to a solid-phase synthesis process of a thymosin alpha 1, belonging to the polypeptide solid-phase synthesis technical field. The invention comprises the following steps: a. a Fmoc-Rink Amide AM resin or a Fmoc-Rink Amide MBHA resin is used as carrier, an H2N-Rink Amide AM resin or an H2N-Rink Amide MBHA resin is obtained after deprotection of the Fmoc; b. side chain carboxyl group of Fmoc-Asp-X is connected with resin amino by the method of solid-phase synthesis to obtain the Fmoc-Asp (resin)-X; c. the left amino acid in the sequence is synthesized in solid-phase with the Fmoc strategy; d. after the amino protection group Fmoc of N terminal amino acid is removed, the N terminal amino acid is acetylated by acetic anhydride and pyridine; e. then the acetylated N terminal amino acid is cut by a cracking agent (tri fluoroacetic acid/ benzoylate sulfide/1, 2- dithioglycol/ Anisole) to obtain the thymosin alpha 1; f. crude product of the thymosin alpha 1 is prepared and separated by HPLC to obtain the pure thymosin alpha 1. The invention can increase significantly the yield of the thymosin alpha 1 and decrease the production cost, which is helpful for scale production and has better industrialization prospect.

The invention relates to a polypeptide synthesis method for octreotide acetate. The method comprises the following steps of: taking chloromethyl resin as a starting raw material, preparing a cesium salt from Boc-Thr(tBu)-OH, sequentially connecting amino acids with protecting groups according to a solid-phase synthesis method so as to obtain protected octapeptide resin, meanwhile, removing Boc protecting groups by sequentially using HCl/isopropyl alcohol, carrying out peptide connecting reaction in a manner of taking DIC and HOBT as condensing agents, carrying out reduction by using palladium carbon/hydrogen gas, meanwhile, cutting off peptide chains so as to obtain reduced octreotide, introducing air at the Ph of 7.8-9 so as to cyclize disulfide linkages, then, obtaining a crude octreotide product, and carrying out separation and purification through a C18 column, thereby preparing a fine octreotide acetate product. The method disclosed by the invention has the advantages that threoninol and Fmoc-threoninol are not adopted, the production cost is very low, the method has large-scale production capacity, the process is stable, the raw and auxiliary materials are convenient to obtain, the production cycle is short, the yield of connected peptide is high, the quality is stable, the use of highly-toxic reagents, such as hydrogen fluoride, trifluoroacetic acid and the like, is avoided, and the pollution caused by waste gas, waste water and waste residues is little.

The invention discloses a method for determining an impurity F in captopril tablets through high performance liquid chromatography and belongs to the technical field of pharmaceutical analysis. Detection is performed under the conditions as follows: an amylase-tris(5-chloro-2-methyl phenyl carbamate) coated chromatographic column is used, normal hexane-absolute ethyl alcohol-trifluoroacetic acid serves as a mobile phase, a volume ratio of the normal hexane to absolute ethyl alcohol to trifluoroacetic acid is 80:20:0.1, a detection wavelength is 215nm, flow velocity is 1ml/min, a column temperature is 35 DEG C and a sample amount is 20[mu]l. A structural formula of the impurity F is as shown in the description. According to the method disclosed by the invention, the content of the impurityF in the captopril tablets can be quantitatively determined, so that the quality of the captopril tablets is effectively controlled. According to the method provided by the invention, the captopril and the impurity F can be proved to be effectively separated in a system suitability solution, and the method has high precision and high separation degree. A signal to noise ratio of a self-contrast solution is more than 10, and if the sample contains the impurity F, the impurity F can be detected.

The invention provides a method for preparing high temperature superconducting thin film by chemical process. The method comprises the following steps: firstly preparing a precursor solution, by mixing Y(CH3COO)3, RE(CH3COO)3, Ba(CH3COO)2 and Cu(CH3COO)2 with ratio of (Y+RE) to Ba to Cu equaling to 1:2:3 (wherein RE is Nd, Sm, Eu, Gd and Dy) and dissolving in 20-30 mol percent aqueous trifluoroacetic acid solution; stirring to be uniform, performing vacuum drying by evaporation to the solvent to obtain gel; then adding methanol, stirring to be uniform, performing drying by evaporation to the solvent to obtain gel; then adding proper amount of methanol to prepare the precursor solution with the total concentration of metal ions of Y, RE, Ba and Cu being 0.8-3.0mol/L; then coating the precursor solution on a substrate; performing low temperature heat treatment at 400-410 DEG C to the coated thin film to decompose trifluoroacetic acid salt; and finally performing high temperature heat treatment at 800-850 DEG C and annealing process at 490-510 DEG C to form YBCO thin film doped with rare-earth element.

The invention belongs to the field of organic chemistry synthesis and particularly relates to a method for preparing 5-fluorouracil. The method comprises the following steps: (1) after nitrogen displacement, adding sodium methoxide into toluene, then dripping part of ethyl formate at first, then dripping methyl fluoroacetate and the rest ethyl formate, and stirring after dripping for reaction; (2) adding methyl alcohol and sodium methoxide, stirring, reducing the temperature to 15-25 DEG C, adding urea for reaction, removing a solvent after reaction, re-adding water, cooling, stirring, regulating the pH to 3-4, and filtering to obtain the product. According to the invention, as ethyl formate and methyl fluoroacetate are mixed and dripped, and the dripping temperature is reduced, loss of ethyl formate is reduced, accordingly, reaction of ethyl formate and methyl fluoroacetate is promoted, and the yield is improved to be more than 74.5%; addition of the solvent is reduced, so that the solvent reclamation amount can be remarkably reduced and the manufacturing cost is greatly lowered.

The invention provides a liquid chromatographic analysis method of L-prolinamide. The liquid chromatographic analysis method comprises the following steps: precisely measuring an L-prolinamide solution, a triethylamine ethanol solution and a derivatization reagent solution respectively, and uniformly mixing through vortex; reacting for a period of time; then adding a diethylamine ethanol solutionand uniformly mixing through the vortex; reacting for a period of time; then adding a trifluoroacetic acid ethanol solution and uniformly mixing through the vortex to obtain an L-prolinamide derivative solution; carrying out chromatographic analysis on the L-prolinamide derivative solution. The liquid chromatographic analysis method provided by the invention can be used for accurately and sensitively detecting the L-prolinamide and D-prolinamide.

The invention provides a synthetic method of silodosin, which is high in yield, simple to operate and safe. The method comprises the following steps: (1) performing acidolysis on a compound shown in a structural formula 4 to obtain a compound shown in a structural formula 2 under the condition that acid used in acidolysis reaction is methylsulfonic acid, trifluoroacetic acid/sulfuric acid, acetic acid/sulfuric acid, polyphosphoric acid or orthophosphoric acid; (2) reacting the compound shown in the structural formula 2 with a compound shown in a structural formula 5 to obtain a compound shown in a structural formula 3; and (3) hydrolyzing the compound shown in the structural formula 3 or salts of the compound to obtain silodosin shown in the structural formula 1, wherein R1 in the structural formulas 2, 3 and 4 is ester groups such as butyryl, valeryl, isobutyryl, benzoyl, p-fluoro benzoyl, p-methyl benzoyl and m-methyl benzoyl; and R2 in the structural formula 5 is good leaving groups such as halogen or sulphonate such as bromine, chlorine, methanesulfonate, benzenesulfonate, p-methyl benzenesulfonate and the like. The method provided by the invention has the advantages that the method is easily-available in raw material and stable and safe in reaction, is convenient to operate, can avoid the reaction conditions which can cause material spraying, and is easy in process control and industrial amplification production.

The invention discloses preparation methods of two types of abiraterone derivatives. The preparation method of a first type of abiraterone derivatives comprises the following steps: by taking ethanediamine as a raw material, carrying out monoprotection on amino by using (Boc)2O, carrying out tertiary amination, and carrying out deprotection of trifluoroacetic acid to obtain N1,N1-di-n-alkyl-1,2-diamine; reacting abiraterone with CDI, then carrying out condensation reaction with the N1,N1-di-n-alkyl-1,2-diamine, and finally carrying out quaternary ammonium salinization reaction to prepare beta-N-methyl-N1,N1-di-n-alkyl carbamic acid-Py-N-methyl -abiraterone ester with different alkane chains. The preparation method of a second type of abiraterone derivatives comprises the following steps: by taking ethanediamine as a raw material, carrying out monoprotection on amino by using (Boc)2O, carrying out tertiary amination, carrying out quaternary ammonium salinization and carrying out deprotection of trifluoroacetic acid to obtain N-methyl-N1,N1-dialkyl ethanediamine; reacting abiraterone with nitrophenyl chloroformate, then carrying out condensation reaction with N-methyl-N1,N1-dialkyl ethanediamine to prepare beta-N-methyl-N1,N1-di-n-alkyl carbamic acid abiraterone ester with different alkane chains. The prepared abiraterone derivatives contain hydrophilic quaternary ammonium salt groups; compared with the abiraterone, the home-made two types of abiraterone derivatives are expected to have high water solubility.

A process for the preparation of an antimicrobial coating solution is described. The process comprises the steps of: (i) mixing a chelating agent with titanium alkoxide and fluoroacetic acid; and (ii) adding an aqueous solution to the mixture from step (i). The antimicrobial coating described is visible light activated. The coating is applied to surfaces and then heat treated to form a transparent layer on the surface. This is particularly advantageous where the surface is glass.

The invention provides an extraction process of small-molecular fucoidan and an application of the small-molecular fucoidan in cosmetics. After kelp is made into kelp wall-broken slurry, a chitosan acetic acid solution is firstly used and is supplemented with sodium perborate to precipitate polysaccharides, and the precipitate is dispersed in distilled water and then is degraded by combining lysozyme with trifluoroacetic acid; and finally, the small-molecular fucoidan is separated by repeated freeze-thaw treatment. The obtained product has low molecular weight (200-300 Da), has high purity, has proper and good fluidity, and can be used for preparing the cosmetics.

The invention belongs to the technical field of fuel cells, and particularly relates to a preparation method of a Schiff base crown ether polymer and application of the Schiff base crown ether polymer in a modified polysulfone anion exchange membrane for a fuel cell. The preparation method comprises the following specific steps: adding trifluoroacetic acid into dibenzo-18-crown-6 and hexamethylenetetramine, so as to obtain dialdehyde dibenzo-18-crown-6; the preparation method comprises the following steps: adding dichloromethane and glacial acetic acid into dibenzo-18-crown-6, and dropwise adding a mixed acid solution of glacial acetic acid and concentrated nitric acid to obtain dinitrodibenzo-18-crown-6; the preparation method comprises the following steps: adding ethanol and an aqueous solution into dinitrodibenzo-18-crown-6 and sodium hydroxide, and then adding thiourea dioxide to obtain diaminodibenzo-18-crown-6; the preparation method comprises the following steps: dissolving dialdehyde dibenzene-18-crown-6 and diaminodibenzene-18-crown-6 into dichloromethane, so as to obtain a target product. The anion exchange membrane prepared by the invention has good alkali-resistant stability and mechanical properties.

The invention discloses a method for determining content and associated substances of sorafenib tosylate. The method comprises the following steps: taking a reverse high-performance liquid phase chromatography, preparing a test solution and a reference solution, respectively measuring 10 micro liters of the test solution and 10 micro liters of reference solution, injecting the solution into a chromatograph, recording a chromatogram, calculating at a peak area according to an external standard method, and drying to complete the test on the content of the sorafenib tosylate and other substances. The method has the advantages that the blank that no method for testing and analyzing the content and associated substances of the sorafenib tosylate is provided at present is filled, the sorafenib tosylate and impurities can be separated by virtue of an acetonitrile-trifluoroacetic acid aqueous solution, the research development and production requirement can be met, and the associated substances in a sorafenib tosylate active ingredient can be more strictly and effectively controlled.

The invention provides a synthesis method of tetracarboxylic dianhydride with a fluorinated rigid structure. According to the method, trifluoromethanesulfonic acid, trifluoroacetic acid and/or sulfuric acid is adopted to replace hydrofluoric acid to serve as a catalyst to achieve conversion from 3,4-dimethylphenol or 3,3',4,4'-tetramethyldiphenyl ether to xanthene tetracarboxylic dianhydride, so that the whole synthesis method has the advantages of being efficient, safe and controllable.

The invention discloses a photocatalytic synthesis method of a C2 substituted 2H-benzothiazole benzylated derivative. The photocatalytic synthesis method comprises the following steps of: mixing 2H-benzothiazole with substituted methyl benzene; adding an oxidizing agent Selectfluor, an additive trifluoroacetic acid and a solvent acetonitrile, carrying out a normal temperature stirring reaction under the protection of nitrogen and the irradiation of an LED blue light lamp, carrying out TLC monitoring until the reaction is finished, and carrying out separation and purification on the reaction liquid to obtain the C2 substituted 2H-benzothiazole benzylated derivative. The new method for synthesizing the C2 substituted 2H-benzothiazole benzylated derivative through visible light induction by taking Selectfluor as an oxidizing agent, trifluoroacetic acid as an additive and acetonitrile as a solvent is high in atom economy, simple in catalytic system, good in product yield, wide in substraterange and suitable for popularization and application.

The invention discloses a preparing method of an energetic crystal material obtained through self-assembly of a melamine nitrogen oxide and an oxidant. The preparing method comprises the steps of 1, preparing the melamine nitrogen oxide, wherein a sufficient amount of melamine is added to an appropriate amount of trifluoroacetic acid to be dissolved, an aqueous hydrogen peroxide solution is addeddropwise, reaction and filtering are conducted to obtain a white precipitate, the white precipitate is dissolved in an appropriate amount of water, alkaline is added to neutralize the solution to keepthe pH value at 7, and filtering is conducted to obtain the melamine nitrogen oxide; 2, preparing the energetic crystal material, wherein the melamine nitrogen oxide is dissolved in the aqueous hydrogen peroxide solution, nitric acid or perchloric acid separately, and through a series of operation, the energetic crystal material obtained through self-assembly of the melamine nitrogen oxide and the oxidant is obtained. The energetic crystal material obtained through self-assembly of the melamine nitrogen oxide with hydrogen peroxide, nitric acid and perchloric acid has the advantages of beingsimple in preparing technology, low in raw material cost, high in density and detonation performance and proper in sensitivity, and is a high-energy explosive with high potential application value.

The invention relates to the technical field of biological chemistry, and particularly discloses a preparation method of fluoroacetamide hapten and application of a monoclonal antibody. The fluoroacetamide hapten is synthesized by taking ethyl fluoroacetate and p-aminophenylacetic acid as main raw materials; the fluoroacetamide hapten and carrier protein bovine serum albumin (BSA) or keyhole limpet hemocyanin (KLH) are coupled through an active lipid method, and thus a conjugate is prepared. Through experimental verification, it shows that the prepared conjugate enables a living body to generate the antibody against fluoroacetamide, that is to say, the prepared conjugate is fluoroacetamide artificial antigen. The prepared fluoroacetamide artificial antigen is suitable for enzyme-linked immunological analysis of fluoroacetamide.

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

The invention discloses a synthesis method of a beta-trifluoromethyl substituted alcohol organic molecule. The method comprises the following steps: firstly, mixing a styrene substrate, sodium trifluoromethanesulfinate and an electrolyte salt lithium perchlorate; adding a solvent ethylene glycol dimethyl ether and a strong acid trifluoroacetic acid while stirring, then inserting a counter electrode below the liquid level of the solvent, and carrying out an electrocatalytic reaction under the conditions of constant current of 15 +/-3 mA and stirring to obtain the beta-trifluoromethyl substituted alcohol organic molecule corresponding to the substrate. The beta-trifluoromethyl substituted alcohol organic molecule is synthesized by using an electro-catalysis means, and an active intermediateis generated through direct initiation of single electron transfer, so the use of a metal catalyst and a peroxidant is avoided, the reaction system is green and efficient, and a practical and effective path is provided for the synthesis of the beta-trifluoromethyl substituted alcohol organic molecule.

The invention discloses a novel synthesis method of methyl fluoroacetate and ethyl fluoroacetate. The method comprises the following specific steps: adding methyl chloroacetate or ethyl chloroacetate into a reaction kettle, and starting stirring; after uniformly stirring, sequentially adding potassium fluoride, a catalyst A and a catalyst B, and closing a charging hole; heating to 120 DEG C by using heat-conducting oil, starting reaction, stopping heating by the heat-conducting oil and starting heat preservation when the kettle temperature reaches 180 DEG C and the kettle pressure reaches 0.8 MPa after 1 hour; after keeping heat preservation for 3 hours and the kettle temperature reaches 220 DEG C and the kettle pressure reaches 1.5 MPa, continuously preserving heat for 5 hours; and cooling to 80 DEG C, discharging, carrying out filter pressing, rinsing, rectifying filtrate through a rectifying tower, and recovering chloroacetate to obtain the product methyl fluoroacetate or ethyl fluoroacetate, the product quality can reach 99.5% or above, and the molar yield (metered by potassium fluoride) reaches 96% or above. The method has the advantages of mild reaction conditions, simple operation, easy control, high fluoro conversion rate, high product yield, simple post-treatment process, realization of solvent-free reaction, and low energy consumption.