35results about How to "Short steps" patented technology

The preparation method comprises the following steps: in the presence of a palladium catalyst, an oxidant, a solvent and a nitrogen-containing heterocyclic ring ligand containing an electron-deficient group, carrying out direct arylation polymerization reaction on aromatic hydrocarbon to be activated and aryl halide to synthesize an anti-nonspecific adhesion polymer in one step; the aromatic hydrocarbon to be activated is a functional monomer containing zwitterionic functional groups; the ligand containing the electron-deficient group is a nitrogen-containing heterocyclic ring ligand; the structural general formula of the prepared non-specific adhesion resistant polymer is # imgabs0 #, R1 and R2 are independent from each other, and n is a natural number greater than 20. The preparation method provided by the invention has the advantages of simple and rapid steps, good stability of functional groups in reaction, and suitableness for industrial production; the non-specific adhesion resistant polymer is high in molecular weight, regular in structure and high in yield, and has a wide application prospect in the field of biological electronic materials.

The invention relates to a synthetic method of a compound 4-hydroxy-2-trifluoromethylpyrimidine, which comprises the following steps: by taking a compound ethyl trifluoroacetate and a compound 3-aminopropanamide as raw materials, firstly converting the raw materials into a compound 3-(2, 2, 2-trifluoroacetamido) propanamide, and then carrying out ring closing reaction to obtain the target compound 4-hydroxy-2-trifluoromethylpyrimidine. The synthetic route has the advantages of short steps, simple operation, low cost, mild reaction conditions, simple post-treatment and ideal yield, and is suitable for process amplification.

The application discloses a synthesis method of 7-bromo-2-chloroquinolin-4-ol, which comprises the following steps: taking 7-bromo-2,4-dichloroquinoline as raw material, converting into 7-bromo-4-(tert-butoxy)-2-chloroquinoline, and reacting under the action of p-toluenesulfonic acid to obtain 7-bromo-2-chloroquinolin-4-ol. The synthesis method of 7-bromo-2-chloroquinolin-4-ol is short in steps, relatively mild in reaction condition, and high in product yield, which not only provides a potential route for the process synthesis of 7-bromo-2-chloroquinolin-4-ol, but also helps the development and utilization of quinoline compounds.

The present invention discloses a method for evaluating bacterial activity based on GelRed dye, wherein metal ions are first mixed with bacterial samples, and then allowed to stand for a certain period of time to obtain a mixed bacterial solution, and then GelRed dye is added to the mixed bacterial solution to mix evenly and then allowed to stand for a certain period of time; ultrapure water is added for centrifugation, the supernatant is discarded, and then Syto9 solution is added for mixing; finally, a fluorescence photometer is used for detection. The evaluation method of the present invention has the characteristics of high sensitivity, rapidity and low toxicity.

The application discloses a synthesis method of 4-hydroxy-5,6-dimethylpyridine-2(1H)-ketone, which comprises the following steps: taking 3-methyl-2,4-pentanedione as raw material, reacting with NaHMDS and dimethyl carbonate, and then regulating the obtained mixed solution to a specific pH value, so as to synthesize the compound 4-hydroxy-5,6-dimethylpyridine-2(1H)-ketone by one-pot method. The synthesis method adopts the cheap 3-methyl-2,4-pentanedione as raw material, realizes one-pot synthesis of the target product, and finally obtains the compound 4-hydroxy-5,6-dimethylpyridine-2(1H)-ketone at low cost, short steps, relatively mild reaction conditions, simple post-treatment and ideal yield.

A method for calculating coordinates of a multi-station fixture of a vertical machining center comprises the following steps: determining a reference point of the fixture and a plurality of stations on the fixture, and measuring the distance between the plurality of stations and the reference point of the fixture to obtain a linear relation between origin coordinates of the plurality of stations and reference coordinates; according to the linear relation between the reference point of the clamp and the zero point of each station, the station zero point coordinate is determined; the linear relation serves as a reference, conversion of a plurality of station coordinate systems is carried out when a machining program is compiled, and the machining zero point of the workpiece to be machined is determined; the clamp is installed on the vertical machining center, and mechanical coordinates of the clamp datum point on the vertical machining center are collected; and inputting the collected mechanical coordinate value of the reference point of the clamp into a vertical machining center system. By means of the method, conversion between the reference coordinate system and the station coordinate system is achieved, on the basis, only coordinate data of the reference original point need to be collected and input into the vertical machining center system when the clamp is replaced every time, and the method is simple in operation step, rapid and high in accuracy.

The invention discloses a synthesis method of 7-bromine-2-chloroquinoline-4-alcohol, which comprises the following steps of: converting 7-bromine-2, 4-dichloroquinoline serving as a raw material into 7-bromine-4-(tert-butoxy)-2-chloroquinoline, and reacting under the action of p-toluenesulfonic acid to obtain the 7-bromine-2-chloroquinoline-4-alcohol. The synthesis method of the 7-bromo-2-chloroquinoline-4-alcohol has the advantages of short steps, relatively mild reaction conditions and high product yield, not only provides a potential route for the process synthesis of the 7-bromo-2-chloroquinoline-4-alcohol, but also contributes to the development and utilization of quinoline compounds.

The aldol condensation reaction catalyst is characterized in that the aldol condensation reaction catalyst contains silicon, oxygen and alkali metal elements and has an amorphous structure, the micropore volume is smaller than 0.05 cm < 3 > / g, the mesopore volume is larger than 0.55 cm < 3 > / g, obvious pore distribution exists in the range of 16-50 nm, the specific surface area is 50-300 m < 2 > / g, the ratio of the mesopore volume to the total pore volume is (0.9-0.99): 1, and the aldol condensation reaction catalyst is represented by an NMR silicon spectrum. The ratio Q4 / Q3 of the height of the signal peak of-113 ppm to the height of the signal peak of-103 ppm is greater than 100, Q4 represents Si (OSI) 4 species, and Q3 represents Si (OSI) 3 (OH) species.

A modified tin-silicon molecular sieve, characterized in that it contains tin, silicon, oxygen and an alkali metal element; the modified tin-silicon molecular sieve is characterized by XPS, the center value of the Sn 3d 5 / 2 spectral peak binding energy is located at 487.1±0.4eV, and the ratio of the spectral peak area of six-coordinated tin to four-coordinated tin is greater than 1:1.

The invention provides a method for preparing an ilastrant intermediate (namely a compound of a formula V or a salt thereof), 4-bromo-3-nitroanisole is used as a raw material of # imgabs0, and (+ / -) 6-(2-amino-4-methoxyphenyl)-5, 6, 7, 8-tetrahydronaphthalene-2-alcohol is obtained through a one-pot Suzuki coupling reaction and reductive hydrogenation. According to the method, the reaction steps are simplified, and the operation process is reduced. Compared with the prior art, the preparation process provided by the invention has the advantages that the obtained product is economic and efficient, the yield and the purity are higher, and the preparation process is more suitable for industrial production; the compound of the formula (V) or the salt thereof can be used for preparing alalisset.

This invention relates to mupirocin compounds, specifically to a method for preparing mupirocin derivatives. The method includes the following steps: 1) benzyloxyheptenol reacts with triethyl orthoacetate via a Claisen rearrangement to generate trans-ethyl olefin ester; 2) the trans-ethyl olefin ester undergoes oxidation to remove debenzylic protection, producing an alcohol compound; 3) the alcohol compound undergoes halogenation to generate a key branched iodide; 4) mupirocin reacts with excess trimethyl orthoformate under acidic catalysis for alcohol protection, followed by ester hydrolysis under alkaline conditions to obtain polyol-protected mupirocin acid; 5) the polyol-protected mupirocin acid reacts with the iodide via a nucleophilic substitution reaction to generate a polyalkyl mupirocin ester; 6) the polyalkyl mupirocin ester undergoes alkaline hydrolysis, followed by acid-base adjustment and deprotection to obtain the crude product, which is then neutralized to acid and purified by slurrying with an inorganic base to obtain the target compound. This invention avoids harsh reaction conditions, has readily available raw materials, high yield, simple operation and purification, and can be used for large-scale production of high-quality target compounds.

The invention discloses a synthetic method of 7-bromo-5, 6-bis (benzyloxy) benzopyrrole and a derivative dimer of the 7-bromo-5, 6-bis (benzyloxy) benzopyrrole. The synthetic method of the 7-bromo-5, 6-bis (benzyloxy) benzopyrrole comprises the following steps: 1) 2-methoxy-5-nitrophenol is subjected to a bromination reaction through NBS (N-bromosuccinimide), and a compound A is obtained; 2) demethylating the compound A to obtain a compound B; 3) performing benzyl protection on two phenolic hydroxyl groups of the compound B to obtain a compound C; and 4) the compound C is subjected to a Baltorry reaction under the action of vinyl magnesium bromide, and the compound is obtained. The invention relates to a synthesis method of 7, 7 '-dimer, which is characterized in that 7-bromo-5, 6-bis (benzyloxy) benzopyrrole is taken as an initial raw material, and the 7, 7'-dimer is obtained through two-step reaction, the synthesis of the 7, 7 '-dimer is reported for the first time, and the synthesis method has the advantages that the raw material is cheap and easy to obtain, the steps are few, the final product is convenient to purify and easy to stably preserve and the like, and the synthesis method of the 2, 7'-dimer is obviously optimized.

The invention discloses a synthesis method of a compound 5-bromo-[1, 1 '-biphenyl]-3-alcohol, and belongs to the technical field of organic synthesis. The synthesis method comprises the following steps: mixing a copper catalyst, alkali, a ligand, 1-phenyl-3, 5-dibromobenzene and a solvent, and stirring to react under the protection of inert gas to obtain a reaction solution; and carrying out post-treatment to obtain the 5-bromo-[1, 1 '-biphenyl]-3-alcohol. According to the invention, the compound 1-phenyl-3, 5-dibromobenzene is used as a raw material, the target compound 5-bromine-[1, 1 '-biphenyl]-3-alcohol is obtained through a copper-catalyzed nucleophilic aromatic substitution reaction and a one-step reaction, the steps are simple and short, the reaction conditions are mild, the post-treatment and purification are simple, an expensive catalyst is not needed, and the method is a novel method for preparing the 5-bromine-[1, 1'-biphenyl]-3-alcohol. And a potential route is provided for large-scale production of 1, 1 '-biphenyl]-3-alcohol.

This invention belongs to the field of fetoglobulin B detection technology, and discloses an immunochromatographic test strip for quantitative detection of fetoglobulin B using quantum dot fluorescent microspheres and its preparation method. The immunochromatographic test strip of this invention includes a sample pad, a release pad, and a nitrocellulose membrane; the release pad is coated with a fetoglobulin B monoclonal antibody labeled with quantum dot fluorescent microspheres and a mouse IgG antibody labeled with quantum dot fluorescent microspheres; the nitrocellulose membrane has a detection line and a control line, the detection line is coated with fetoglobulin B monoclonal antibody, and the control line is coated with goat anti-mouse IgG antibody. The immunochromatographic test strip of this invention reduces the detection time to 9-12 minutes, and the total detection time is only 20 minutes, achieving rapid and accurate quantitative detection of fetoglobulin B. It also features high detection sensitivity, a wide detection range, and simple and rapid operation, which is beneficial for the screening and monitoring of atherosclerotic coronary heart disease.

The present invention belongs to the technical fields of organic synthesis, fine chemicals and pharmaceutical synthesis, and specifically relates to a method for preparing γ-vinylidene-butenoic acid lactones and / or benzofulvene compounds. The method utilizes an acid-catalyzed dehydration rearrangement reaction of cyclopropenyl alcohol derivatives to achieve the synthesis of two important compounds, γ-vinylidene-butenoic acid lactone and benzofulvene, under the condition of a "one-pot reaction"; at the same time, the preparation method is used as an important synthesis strategy to achieve the efficient synthesis of the anti-inflammatory drug rofecoxib and the benzofulvene natural product anmindenol A.

This invention discloses a method for synthesizing an aromatic formate ester compound, comprising: Step S1: adding a photosensitizer, a base, an organic solvent, an aryl alkyne, and an organic bromide as reactants into a reaction vessel; Step S2: placing the reaction vessel under visible light irradiation and stirring the reaction vessel under a preset temperature range and atmospheric conditions; Step S3: monitoring the reaction progress, and after the reaction is completed, concentrating the reaction solution under vacuum to remove volatile solvents, and then purifying the reaction solution using column chromatography to obtain the aromatic formate ester compound. The method for synthesizing an aromatic formate ester compound provided by this invention is more environmentally friendly and economical than traditional esterification reactions, and is also highly efficient and simple to operate.

The application discloses a diflunisal derivative, a preparation method and application thereof, and belongs to the technical field of agricultural fungicides. The preparation method comprises the following steps: mixing 2', 4'-difluoro-4-hydroxy-[1, 1'-biphenyl]-3-carboxylic acid, a condensing agent and an organic base in an ice bath and an inert organic solvent, and activating for 10-30 minutes; then adding an amine compound with a general formula of R-NH2, and stirring and reacting at room temperature for 20-28 hours; after the reaction is completed, extraction, washing, drying, concentration and column chromatography purification are performed, so that the target diflunisal derivative is obtained. The compound disclosed by the application has a novel structure, shows excellent inhibitory activity on cucumber botrytis cinerea, rice pellicularia sasakii, brassica rapa sclerotium, wheat fusarium graminearum and other plant pathogenic fungi, can be used as an active ingredient for preparing an agricultural fungicide or a fungicide composition, and provides a new lead structure for developing a new succinate dehydrogenase inhibitor fungicide.

A method for synthesizing a substituted nitrogen-containing quinazolinone compound is implemented by using a reinforced heating jacket, using trans-3(3-pyridyl)allylic acid, 2-(7-azabenzotriazole)-N,N,N',N'-tetramethyluronium hexafluorophosphate and ethyl 2-aminobenzoate as raw materials; and finally obtaining the product (E)-3-(4-chlorobenzyl)-2-(2-(pyridin-3-yl)vinyl)quinazolin-4(3H)-one.

The invention discloses a method for synthesizing diaminopyrimidine nitrogen oxide, which comprises: performing a ring-closing reaction on ethoxymethylene cyanoacetoethyl ester and guanidine in a reaction solvent to obtain a pyrimidine skeleton intermediate, performing a decarboxylation reaction in a decarboxylation reagent and an organic solvent to obtain a diaminopyrimidine intermediate, and reacting with an oxidant to obtain diaminopyrimidine nitrogen oxide. The invention uses ethoxymethylene cyanoacetoethyl ester and guanidine as raw materials, sequentially undergoes a ring-closing reaction, a hydrolysis decarboxylation reaction and an oxidation reaction to obtain diaminopyrimidine nitrogen oxide in high yield. The synthetic route is novel, and a new synthetic method is provided for 2,4-diaminopyrimidine and 2,4-diaminopyrimidine nitrogen oxide. The raw materials are cheap and easy to obtain, the cost is low, and operations such as pressurization are not required, and a synthetic route with simple operation, short steps, high reaction selectivity and good safety is provided.

The invention discloses a synthesis method of an important intermediate 3 ', 5'-dichloro-2, 2, 2-trifluoroacetophenone of fluralana, and the synthesis route is as follows: # imgabs0 #. The preparation method has the advantages of short steps, low price of reaction raw materials, milder process conditions, small amount of three wastes, high reaction yield and good product quality, has better competitive advantages, and meets the requirements of modern industrial mass production.

The invention belongs to the technical field of chemical synthesis of drugs, and particularly discloses a novel synthetic route of an anti-hyperuricemia drug dotinirad (Dotinirad, the CAS number is 1285572-51-1, and the chemical name is 3-(3, 5-dichloro-4-hydroxybenzoyl)-1, 1-dioxo-2, 3-dihydro-1, 3-benzothiazole). The invention further discloses a preparation method of the dotinirad, the CAS number is 1285572-51-1, and the chemical name is 3-(3, 5-dichloro-4-hydroxybenzoyl)-1, 1-dioxo-2, 3-dihydro-1, 3-benzothiazole. According to the route, p-hydroxybenzoic acid which is low in price and easy to obtain serves as a starting raw material, a target product is obtained through four-step reaction of chlorination, acylating chlorination, amide condensation and oxidation, the method has the advantages of being short in step, mild in condition and high in yield, use of 2-aminothiophenol which is odorous and unstable is avoided, benzothiazole which is more stable and low in price is used as a raw material, and the method is suitable for industrial production. The concept of green chemistry is met. The industrial production cost is remarkably reduced, and an efficient and reliable technical scheme is provided for large-scale production of the dotenorad.

The present invention relates to the field of pharmaceutical technology, and in particular to a preparation method of a benzimidazole pharmaceutical intermediate. The preparation method comprises the following steps: in a solvent system, 3-amino-2-chlorobenzoic acid methyl ester and ethyl formate are heated and reacted under the action of a catalyst to obtain a 2-chloro-3-((ethoxymethylene)amino)benzoic acid methyl ester solution, wherein the catalyst is p-toluenesulfonic acid or glacial acetic acid; 4'-(aminomethyl)-[1,1'-biphenyl]-2-nitrile and a nitrogen oxide catalyst are added to the 2-chloro-3-((ethoxymethylene)amino)benzoic acid methyl ester solution, and then the reaction is carried out under oxygen conditions. After the reaction is completed, the benzimidazole pharmaceutical intermediate is obtained by post-processing. The preparation method has mild reaction conditions, simple operation, short route, is environmentally friendly, has high product quality yield, and is suitable for commercial production.

The invention discloses a method for separating ceramide from hydrated degumming by-products, which comprises the following steps: (1) adding a certain amount of C1-C3 alcohol or C3-C5 ketone solvent into the hydrated degumming by-products containing ceramide to ensure that the concentration of alcohol or ketone in the system is more than or equal to 30%, centrifuging and collecting precipitate; and (2) adding 80%-100% by volume of C1-C3 alcohol or C3-C5 ketone solvent into the precipitate obtained in the step (1) for extraction, separation and concentration of a supernatant to obtain a ceramide product. The content of ceramide separated by the method can reach 9% or above, efficient conversion of byproducts is achieved, and the comprehensive utilization rate of resources is greatly increased.

The invention relates to a synthesis method of a compound 6-chloro-3-fluoro-2-iodopyridine, which is characterized in that a compound 2-chloro-5-fluoropyridine is used as a raw material, and is converted into a target compound 6-chloro-3-fluoro-2-iodopyridine in a high-selectivity manner through a one-step reaction. The synthesis method is low in cost, short in step, relatively mild in reaction condition, high in reaction selectivity and high in product yield, not only provides a potential route for process synthesis of 6-chloro-3-fluoro-2-iodopyridine, but also contributes to development and utilization of pyridine compounds.

According to the process reaction, N-Cbz-4-oxo-3-pyrrolidine ethyl formate and a Wittig reagent of ethyl triphenyl phosphorus iodide are used as synthesis starting points, firstly, N-Cbz-4-oxo-3-pyrrolidine ethyl formate and the Wittig reagent of ethyl triphenyl phosphorus iodide are subjected to nucleophilic addition to generate olefin reaction, then the olefin reaction is subjected to hydrolysis reaction under the alkaline condition to generate acid, and the acid is subjected to acid hydrolysis reaction under the alkaline condition to generate the N-Cbz-4-oxo-3-pyrrolidine ethyl formate and the Wittig reagent of ethyl triphenyl phosphorus iodide. The method is reasonable in process, high in yield, simple to operate, low in production cost and beneficial to large-scale industrial production, and fills up the process blank in related fields.

An alkali metal modified titanium silicalite molecular sieve is characterized in that the molecular sieve contains titanium, silicon, oxygen and alkali metal elements, a Raman spectrum of a 325nm light source is used for characterizing that a titanium species signal peak exists in a range of 990cm <-1 > + / -20cm <-1 >, no obvious titanium species signal peak exists in a range of 1125cm <-1 > + / -20cm <-1 >, a molecular sieve skeleton structure signal peak exists in a range of 800cm <-1 > + / -20cm <-1 >, and the peak area is calculated as intensity. And the ratio I (90) / I (800) of the signal peak intensity of 990 + / -20 cm <-1 > to the signal peak intensity of 800 + / -20 cm <-1 > is (0.2-2): 1.

The process described in this application uses ethyl N-Cbz-4-oxo-3-pyrrolidinecarboxylate and Wittig reagent ethyltriphenylphosphine iodide as the starting points for synthesis. First, ethyl N-Cbz-4-oxo-3-pyrrolidinecarboxylate undergoes a nucleophilic addition reaction with Wittig reagent ethyltriphenylphosphine iodide to generate an olefin. Then, it undergoes a hydrolysis reaction under alkaline conditions to generate an acid, followed by a double bond reduction reaction under catalytic hydrogen conditions. The process is reasonable, has high yield, is simple to operate, and has low production cost, which is conducive to large-scale industrial production and fills a technological gap in related fields.

The invention provides a synthesis method of asymmetric amino urea (V), which comprises the following steps: directly activating an amine compound (I) by a phenyl chloroformate compound (II) to obtain a carbamate compound (III), and directly reacting the carbamate compound (III) with an amine compound (IV) to obtain the asymmetric amino urea (V). According to the invention, the compound phenyl chloroformate compound (II) is introduced, two molecules of different amine compounds are activated to directly form asymmetric urea, the process adopts a one-pot method, the steps are relatively short, the operation is simple, and the cost is low. R < 1 > and R < 2 > are respectively and independently C1-C6 alkyl groups, aryl groups and heterocyclic rings; r is hydrogen, C1-C6 alkyl, aryl, heterocyclic ring, halogen or nitryl.

An alkali metal-modified titanium-silicon molecular sieve, characterized in that the molecular sieve contains titanium, silicon, oxygen, and alkali metal elements, and is characterized by Raman spectroscopy using a 325 nm light source, showing a value at 990±20 cm⁻¹. ‑1 A titanium species signal peak exists within the range, at 1125±20 cm⁻¹. ‑1 No obvious titanium species signal peak was observed within the range of 800±20 cm⁻¹. ‑1 A molecular sieve framework structure signal peak exists within the range, calculated with peak area as intensity, 990±20 cm⁻¹. ‑1 Signal peak intensity and 800±20cm ‑1 The ratio of signal peak intensity I(990) / I(800) is (0.2-2):1.

The utility model relates to the technical field of new energy automobile main shells, in particular to a main shell for a new energy automobile, which comprises a support frame, a top plate I arranged on one side of the top of the support frame, a clamping plate I arranged on the top plate I, a top plate II arranged on the other side of the top of the support frame, and a flange extending outwards arranged at the bottom of the support frame. A main plate is installed at the front end of the supporting frame, a second clamping plate and a third clamping plate are arranged on the second top plate, a plurality of protruding blocks are arranged at the bottoms of the first top plate and the second top plate, a partition plate is further arranged between the first top plate and the second top plate, a plurality of first reinforcing plates are arranged between the supporting frame and the turned-over edge, and a plurality of second reinforcing plates are arranged between the first top plate and the supporting frame. According to the utility model, the percent of pass of products is improved by reducing air shrinkage holes, the structural strength is high, the safety and durability are strong, the structural design is simple, the battery is convenient to maintain and replace, the maintenance cost is reduced, and the operation steps of disassembly and replacement are fast.