61results about How to "Few reaction steps" patented technology

The invention discloses a polyethylene glycol-poly (2-vinyl) ethylene glycol copolymer and a preparation method thereof, and relates to the technical field of high polymer materials, and the structure of the polyethylene glycol-poly (2-vinyl) ethylene glycol copolymer is selected from any one of the following structural formulas: # imgabs0. The preparation method comprises the following steps: taking hydroxyl-containing polyethylene glycol and 4-vinyl-1, 3-dioxocyclopent-2-ketone or vinyl ethylene oxide as raw materials; under the action of a palladium catalyst and a phosphine ligand, the polyethylene glycol-poly (2-vinyl) glycol copolymer is efficiently prepared and can be used in the fields of hydrophilic / hydrophobic materials, drug carriers, antibacterial materials, phase change materials, shape memory materials and the like.

A method for preparing a 4,4'-dihydroxybiphenyl compound relates to a method for preparing an organic compound. The method uses 2,6-di-tert-butylphenol as a raw material and a new copper complex as a catalyst to efficiently generate 3,3',5,5'-tetra-tert-butylbiphenyl, which is de-tert-butylated to generate 4,4'-dihydroxybiphenyl. 4,4'-dihydroxybiphenyl is an important organic intermediate, often used as a rubber antioxidant and plastic antioxidant, for colorless vulcanized rubber products, rubber products for food packaging and medical latex products, and also for sulfur chloride cold vulcanized products, such as medical gloves. At the same time, it is also a dye intermediate and a stabilizer for petroleum products, such as a stabilizer for synthetic photosensitive materials and lubricating greases. In terms of synthetic polymers, due to its excellent heat resistance, it is often used as a modified monomer for polyesters, polyurethanes, polycarbonates, polysulfones and epoxy resins, etc., to manufacture excellent engineering plastics and composite materials.

The invention discloses a preparation method of oxilafluorine, which comprises the following step: carrying out alkylation, deprotection, hydroxyethylation and salt forming reaction on a compound (II) to prepare the oxilafluorine as shown in a formula (I). The method has the advantages of low raw material cost, simple process operation, environmental friendliness, high reaction yield, high product purity and wide industrial prospect.

The invention belongs to the technical field of organic synthesis of pesticides, and discloses a synthesis method of pyroxasulfone. The synthesis method of pyroxasulfone comprises the following steps: taking an intermediate A as shown in a formula (I) and a sulfonating agent, and adding a catalyst for reaction to obtain an intermediate B as shown in a formula (II); taking the intermediate B and an intermediate C as shown in a formula (III), and reacting under an alkaline condition to obtain pyroxasulfone. According to the synthesis method of pyroxasulfone, reaction steps are reduced, and the process duration and the production period of pyroxasulfone are greatly shortened; the used raw materials are low in cost and easy to obtain, the reaction conditions are mild, and oxidants such as hydrogen peroxide are not needed; meanwhile, few three wastes are generated in the technological process, and the method is environmentally friendly, is suitable for green large-scale production, and is a green synthesis method which is efficient, environmentally friendly and easy to control.

The invention discloses a preparation method of N, N-diethyl alkyl amidine, which comprises the following steps: dissolving N-long-chain alkyl methyl acetimidate and diethylamine in an organic solvent, heating the organic solvent to 20-100 DEG C, reacting at normal pressure for 0.1-100 hours, reducing the pressure of the organic solvent to 0.01-0.08 MPa, reacting at 20-120 DEG C for 0.1-24 hours, and stopping the reaction to obtain the N, N-diethyl alkyl amidine. The N, N-diethyl alkyl amidine is obtained by dissolving the N-long-chain alkyl acetimidic acid methyl ester and the diethylamine in the organic solvent to react, the used raw materials are easy to obtain, the preparation method is simple, the reaction steps are few, operation is easy, toxic and harmful reagents are not needed in the reaction process, environment friendliness is achieved, and the obtained N, N-diethyl alkyl amidine is high in yield, good in purity and suitable for industrial production. The method is suitable for large-scale industrial production, has a wide application prospect, and can be used as a surfactant and a drug synthesis intermediate.

The invention relates to a novel pure organic multiple illuminant based on aryl carbazole and a preparation method thereof. The reaction structural formula is shown in the specification. The preparation method comprises the following steps: stirring a mixture of 4-bromo-4 '-iodobiphenyl or 2, 6-dibromonaphthalene, carbazole, K2CO3, copper powder and a solvent DMF (Dimethyl Formamide) under nitrogen to react; extracting, drying, filtering and performing rotary evaporation to obtain a crude product; mixing and reacting the obtained crude product, 4-hydroxybenzonitrile, Cs2CO3, CuBr, a ligand 1-(2-pyridyl)-2-acetone and a solvent DMSO (Dimethylsulfoxide); 4-[4 '-(9H-carbazole-9-yl)-4-biphenyloxy] benzonitrile or 4-[6-(9H-carbazole-9-yl)-2-naphthyloxy] benzonitrile with the instant fluorescence-delayed fluorescence-room temperature phosphorescence triple emission characteristic is obtained through drying, filtering, rotary evaporation, separation and purification. The method has good application potential in the fields of anti-counterfeiting, information encryption, organic light-emitting diodes, biosensing imaging and the like. # imgabs0 #

The invention relates to blood concentration detection, in particular to a reagent and a method for detecting a monoclonal antibody drug and an anti-monoclonal antibody drug antibody. The reagent for detecting the monoclonal antibody drug and the anti-monoclonal antibody drug antibody comprises a reagent C and a reagent D, wherein the reagent C comprises a mouse anti-F (ab) 2 monoclonal antibody-1 coupling luminous marker and mouse anti-F (ab) 2 monoclonal antibody-2 coupling biotin; the reagent D comprises a macromolecular monoclonal antibody drug coupled luminous marker and F (ab) 2 coupled biotin; the mouse anti-F (ab) 2 monoclonal antibody-1 coupling luminous marker and the macromolecular monoclonal antibody drug coupling luminous marker are mouse anti-F (ab) 2 monoclonal antibody-1 and macromolecular monoclonal antibody drugs which are marked by luminous markers. According to the invention, the monoclonal antibody drug and the anti-drug antibody thereof can be simultaneously detected by one sample, the reaction steps are fewer, and the reaction time is shorter.

The invention provides a polycaprolactone-poly (2-vinyl) ethylene glycol copolymer and a preparation method thereof.The preparation method comprises the steps that raw materials are provided, and the raw materials comprise polycaprolactone containing 1-4 hydroxyl groups and further comprise 4-vinyl-1, 3-dioxocyclopent-2-ketone or vinyl ethylene oxide; the preparation method comprises the following steps: dissolving the raw materials in an organic solvent, and reacting in the presence of a palladium catalyst and a phosphine ligand to obtain the polycaprolactone-poly (2-vinyl) ethylene glycol copolymer. The preparation method disclosed by the invention has the advantages of high efficiency and high selectivity, and the prepared copolymer is relatively high in vinyl content, controllable in molecular weight and narrow in molecular weight distribution.

The application discloses a method for synthesizing tervalent tetraaryl iron porphyrin from pyrrole, aromatic aldehyde and ferrous salt, which comprises the following steps: adding anhydrous aluminum chloride, aromatic aldehyde, pyrrole and ferrous salt into DMF under stirring, and then heating and refluxing the reaction mixture for 0.5 hours under nitrogen; removing the nitrogen and continuing to heat the reaction mixture for a certain time; stopping the reaction; cooling the reaction mixture; and placing the reaction mixture at 273K overnight; and finally filtering the reaction mixture to obtain the iron porphyrin.

The invention discloses a method for preparing phenyl acetate with high selectivity. A phosphoric acid solution is added into a magnesium chloride solution, stirring and heating are performed to obtain a suspension, the suspension is dried to constant weight to obtain a white solid, the white solid is ground to obtain powder, and the powder is calcined to obtain the catalyst. Then mixing phenol and a catalyst, placing the mixture in an oil bath for reflux reaction, dropwise adding acetic anhydride, distilling after the reaction is finished, and collecting a fraction at 190-195 DEG C, namely phenyl acetate. According to the magnesium chloride loaded phosphoric acid type catalyst (MgCl2-H3PO4) prepared by the method disclosed by the invention, phenol and acetic anhydride react without a solvent, MgCl2-H3PO4 is a solid catalyst, can be recycled only by filtering and can be repeatedly used after being washed, and MgCl2-H3PO4 also improves the selectivity of phenyl acetate and reduces the production cost.

This invention provides a method for preparing 4,1-disubstituted pyrrolo[1,2-a]quinoxaline-1-yl ketone derivatives, belonging to the field of organic synthesis technology. This invention uses 2-(1H-pyrrolo-1-yl)aniline compounds and α-carbonyl acids as reactants, employing only ammonium persulfate as an oxidant. Under metal-free catalysis, a one-pot tandem reaction is carried out to simultaneously complete the cyclization of the pyrrolo[1,2-a]quinoxaline nucleus and the C-1 acylation modification. The substituents at the 4- and 1-positions of the product can be flexibly controlled by changing the α-carbonyl acid with different structures. This method requires no pre-modified substrate, eliminates the need for metal catalysts, avoids the risk of metal residue, and features simplified steps and high functional group compatibility, providing a new green and low-cost route for the synthesis of polysubstituted pyrrolo[1,2-a]quinoxaline ketone derivatives.

The application discloses a preparation method of a trans-7H-pyrrolo[2,3-d]pyrimidine compound, and the full name of the trans-7H-pyrrolo[2,3-d]pyrimidine compound is trans-N-methyl-4-(methyl-7H-pyrrolo[2,3-d]pyrimidin-4-ylamino)cyclohexylmethanesulfonamide maleate, which is prepared from trans-4-[(tert-butoxycarbonyl)amino]cyclohexane carboxylic acid and 4-chloro-7H-pyrrolo[2,3-d]pyrimidine as starting materials through reduction, chlorination, substitution, oxidation, methylation, condensation and salt formation reactions. The preparation method has the advantages of few reaction steps, simple operation, low production cost, high production efficiency, high yield, high product purity and suitability for scale-up production.

The invention provides a polyphenylene ether polyol terminated with an alcohol hydroxyl group and a preparation method thereof. The polyphenylene ether polyol terminated with an alcohol hydroxyl group is prepared by reacting a double-terminated hydroxyl polyphenylene ether with an alkyl carbonate or an epoxide in the presence of an alkaline catalyst, and has alcohol hydroxyl groups at both ends. The molecular weight and degree of polymerization of the polyphenylene ether polyol terminated with an alcohol hydroxyl group are adjustable, and the property is stable. The polyphenylene ether polyol terminated with an alcohol hydroxyl group can be used not only to modify a polymer, but also as an intermediate for preparing a polymer. The addition of the polyphenylene ether polyol terminated with an alcohol hydroxyl group can give the obtained product some unique characteristics of polyphenylene ether, and improve the hardness, heat resistance and other properties of the obtained polymer. At the same time, the preparation method of the polyphenylene ether polyol terminated with an alcohol hydroxyl group is simple, the reaction selectivity is high, the yield is high, the production cost is low, and the application prospect is good.

The invention discloses photocatalytic stereoselective E-type olefination of alkynyl amide and a preparation method of the alkynyl amide. The method is carried out in a water-phase micelle reaction system and is completed under the driving of visible light. According to the method, an alkynyl amide compound is taken as a raw material, sodium ascorbate is taken as a green reducing agent, Ru (bpy) 3 (PF6) 2 or [Ir (dtbpy) (ppy) 2] PF6 is taken as a photocatalyst in a water-phase micelle environment formed by a surfactant lauryl sodium sulfate (SDS), and under the protection of inert gas, catalytic circulation is initiated by visible light irradiation at 20-40 DEG C, so that the alkynyl amide compound is highly selectively converted into an E-type olefin product. The method is mild in condition, simple in step, high in stereoselectivity, environment-friendly and safe to operate, the problem that flammable and explosive reagents or harsh reaction conditions need to be used in a traditional method is solved, and a green and efficient preparation way is provided for preparation of the E-type acrylamide compound.

The invention relates to the technical field of medical instruments, in particular to a heparin coating based on material surface ammonification modification and a preparation method thereof, and the preparation method at least comprises the following steps: carrying out ultrasonic pretreatment on a base material with purified water, and drying for later use; the preparation method comprises the following steps: performing amination modification on a base material subjected to ultrasonic pretreatment by adopting an ammoniation reagent solution, and immersing the base material into a heparin solution to prepare the base material with a heparin coating on the surface. The surface of the material is subjected to amination modification by adopting a micromolecular ammoniation reagent and / or a macromolecular ammoniation reagent system, complex pretreatment such as plasma and ultraviolet rays does not need to be carried out on a base material, specific functional group activation does not need to be carried out on heparin, and the heparin is directly reacted after being subjected to ammoniation modification; the stable covalent grafted heparin anticoagulation coating can be formed, the anticoagulation time is prolonged, and the long-term implantation requirement is met.

The invention discloses a polymer modified asphalt composition and a preparation method thereof, and relates to the technical field of asphalt materials. The invention has the advantages that the performance of the asphalt composition is improved through composite modification of multiple components, the surface activity of nano silicon dioxide is enhanced after pretreatment, the gaps between asphalt molecules are filled, the structural stability and wear resistance are improved, and the nano silicon dioxide is tightly combined with the asphalt molecules due to its nano size, the plant polymerizable components extracted from flax seeds are subjected to a series of treatments, and the active groups thereof react with the asphalt molecules to improve the flexibility and adhesion, the ionic liquid is synthesized and pretreated, and the anions and cations act on the active sites of the asphalt molecules to improve the anti-aging performance, the thermosensitive polymer is composed of a copolymer containing specific chain segments, the low-temperature shrinkage makes the molecular structure compact and crack-resistant, and the high-temperature stretching adapts to the volume expansion and remains stable, effectively improving the high-temperature stability and low-temperature crack resistance, and extending the service life of the paved material.

The invention provides a synthesis process of metaraminol bitartrate, which adopts N-benzyloxycarbonyl-L-alanine and 3-benzyloxybromobenzene as initial raw materials at the same time, is low in cost and easy to obtain, not only can reduce reaction steps, but also can avoid the risk of impurity increase caused by parent nucleus synthesis, can adopt a conventional accurate method to perform quality control, and is suitable for industrial production. And the method is good in process reproducibility and suitable for commercial production. The metaraminol bitartrate obtained by the synthesis method disclosed by the invention has the advantages of high total yield (up to 80%), high purity (up to 99.993%), low total impurity content, low non-specific single impurity content, no impurity A or impurity B detected, and no diastereoisomer detected. According to the synthesis method, an enzyme catalyst and an expensive catalyst are not used, the requirement for equipment is low, implementation is easy, reaction operation is easy to control, mildness, safety and reliability are achieved, needed reagents are environmentally friendly, and a foundation can be laid for later industrial enlarged production.

The application provides a preparation method of imatinib mesylate, wherein 4-(4-methylpiperazin-1-yl)methyl benzoic acid dihydrochloride (compound 5) is neutralized by sodium hydroxide to be free, then directly subjected to condensation with N-(5-amino-2-methylphenyl)-4-(pyridin-3-yl)pyrimidin-2-amine (compound 4) to obtain imatinib, and then the imatinib is subjected to salt formation with methanesulfonic acid to obtain imatinib mesylate. The preparation method is safe and environment-friendly, simple and convenient to operate, low in cost and has industrialization value.

This invention discloses a highly efficient oxygen removal reagent and its application in the deoxygenation reconstruction of carbon resource molecular skeletons, comprising a pivot reagent, a phosphine reagent, an azo reagent, a reducing agent, an acid reagent, a base reagent, a photosensitizer, and an organic solvent; wherein, X in the pivot reagent includes a hydrazine group or a sulfone group; PG is a protecting group; LG is a leaving group; by using natural oxygen-containing functional groups such as alcohols, aldehydes, and ketones as direct coupling precursors, an integrated in-situ activation-deoxygenation coupling process is achieved, significantly reducing reaction steps.

This invention discloses a deuterated scintillator with a space charge transfer structure, its preparation method, and its application in X-ray scintillation imaging, belonging to the field of scintillator materials. The scintillator structure of this invention is characterized by using tripterene as a bridging unit to connect a planar nitrogen-oxygen donor and a deuterated boron-oxygen acceptor. While ensuring high X-ray absorption capacity, it reduces the non-radiative transition rate, achieving a synergistic effect of high luminescence quantum yield, fast decay lifetime, and low self-absorption, thus meeting the requirements of high-resolution, high-sensitivity X-ray imaging. A transparent and highly flexible organic gel scintillator film is prepared by blending and polymerizing an X-ray-responsive organic scintillator with hydroxyethyl methacrylate. This film exhibits highly efficient luminescence under both photoluminescence and radiative luminescence conditions, significantly improving X-ray imaging sensitivity and resolution. Experiments show that the organic gel scintillator film prepared by this invention achieves a resolution of over 16.0 lp / mm under standard line-pair cards.

The invention discloses a synthesis process of alkali metal trialkyl borohydride. A synthesis process of alkali metal trialkyl borohydride comprises: alkali metal borohydride and olefin are subjected to addition reaction in an organic solvent to prepare alkali metal trialkyl borohydride. Compared with the prior art, the synthesis process of alkali metal trialkyl borohydride provided by the invention does not need to prepare and purify sensitive intermediate trialkyl boron, has high yield of target product, has few reaction steps, strong operability, and easy to obtain raw materials, and is suitable for industrialized scale-up production.

The invention relates to the field of chemical synthesis, in particular to a three-component electrochemical synthesis method of dithiophosphonate. According to the invention, a trivalent phosphine hydrogen compound, elemental sulfur and mercaptan / phenol three-component electrochemical oxidation reaction system is constructed, and a series reaction is carried out to synthesize the phosphorus and sulfur-containing dithiophosphonate derivative in one step. The method is simple, convenient and safe in reaction operation, mild in reaction condition, simple and efficient, free of obvious by-products, relatively high in tolerance of compound functional groups, convenient in post-treatment, generally relatively high in yield, wide in substrate applicability, simple to operate and capable of avoiding the use of highly toxic thiophosphoryl chloride and foul Lawesson reagents, and can be used for large-scale synthesis.

The invention belongs to the technical field of medicine synthesis, and particularly relates to a synthesis method of a ketorolac intermediate. The ketorolac intermediate 5-benzoyl pyrrole-2-methane triethyl tricarboxylate is synthesized by taking 2-benzoyl pyrrole as a starting material. The method has the advantages of single reaction catalyst, simple operation, few reaction steps and high product yield, avoids the problem that a large amount of manganese ions and acetic acid exist in the system in the prior art, and is suitable for industrial large-scale production.

The invention discloses a preparation method of 2, 6-di-tert-butyl-4-phenyl-2, 5-cyclohexadienyl-1-one, which comprises the following steps of: adding a catalyst and a catalyst into a reaction kettle; relates to the field of organic synthesis. The 2, 6-di-tert-butyl-4-phenyl-2, 5-cyclohexadienyl-1-ketone is prepared by taking secondary amine as a catalyst, taking 2, 6-di-tert-butylphenol and benzaldehyde as raw materials and taking di-n-butylamine as a catalyst and adopting a one-pot boiling mode, the conversion rate of the main raw materials in the whole reaction stage reaches 98%, the product purity reaches 99.5%, and the yield of the 2, 6-di-tert-butyl-4-phenyl-2, 5-cyclohexadienyl-1-ketone is high. The preparation method has the advantages of high raw material utilization rate, high product yield, less waste and environmental protection. Secondly, the sulfonic acid modified zeolite is subjected to acid steam roasting treatment, so that groups of the sulfonic acid modified zeolite are uniformly distributed on the surface and in pores of the zeolite, and the thermal stability and the chemical stability of the modified zeolite are effectively improved; the liquid exchanged by the sulfonic acid modified zeolite is distilled and purified to recover the di-n-butylamine, so that the loss rate of the di-n-butylamine sulfate is further reduced, the recovery rate is up to 95-97.1%, and the purposes of feeding the next batch and recycling are achieved.

The present application relates to a preparation method of CL2A-SN-38, the preparation method comprises the following steps: (1) reaction of intermediate 3 and compound 2 to prepare intermediate 4; (2) dehydroxy protection group and then deamination protection group of intermediate 4 prepared in step (1) to prepare the CL2A-SN-38. The preparation method of CL2A-SN-38 has the advantages of few reaction steps, simple operation, low cost, high purity and yield, and is suitable for industrial production.

The invention provides a fenerenone key intermediate and a preparation method thereof, and relates to the technical field of medicine synthesis. The invention relates to a preparation method of a fenerenone key intermediate, which comprises the following steps: by taking 4-methylbenzonitrile as a raw material, sequentially carrying out halogenation, alkaline hydrolysis and nucleophilic substitution reaction to obtain 4-cyano-2-methoxybenzaldehyde. The preparation method of the fenerenone key intermediate provided by the invention is simple and convenient to operate, green, environment-friendly, high in product yield and suitable for industrial production.

The application discloses a preparation method of S4-(2-cyanoethyl)-4-thiothymine deoxyriboside monomer, and 5'-O-DMT-uridine is used as a starting material. First, the starting material is reacted with a sulfonylation reagent to generate a sulfonylation reaction on a carbonyl group at a 4 position of the starting material to obtain compound II. Then, the compound II is reacted with 3-mercapto propionitrile to continuously generate a substitution reaction on the 4 position to obtain compound III. Finally, the compound III is reacted with a phosphorus reagent to obtain the S4-(2-cyanoethyl)-4-thiothymine deoxyriboside monomer. The method does not need to protect a 3'-hydroxyl group, has a shorter reaction route, milder reaction conditions, and high synthesis efficiency.

The invention discloses a method for synthesizing a tetrahydroquinoline compound with a C-B bond, comprising the following steps: mixing an Rh-type catalyst, a phosphorus ligand or an NHC ligand and a solvent, adding borane, quinoline or a derivative thereof, reacting, cooling to 0-5°C, adding an acylating agent and a base, warming to room temperature, reacting again, and obtaining a tetrahydroquinoline compound with a C-B bond. The synthetic method of the present invention is a two-step one-pot method, using metal Rh as a catalyst, and in the absence of the need for pre-substrate activation, performing two dearomatization reduction reactions of quinoline with high chemical selectivity, high regio- and stereoselectivity under mild conditions, and realizing two hydroborations of quinoline in one step, and obtaining a tetrahydroquinoline compound with a C-B bond. The substrate of the method is widely applicable, and the functional group has good tolerance, and the corresponding tetrahydroquinoline compound containing a chiral C-B bond can be obtained by using a chiral ligand.

Disclosed is a method for preparing paraxylene by biomass conversion, comprising the following steps: (1) contacting a biomass starting material with a hydrogenation catalyst for reaction in a multiphase system formed by an organic solvent, an inorganic salt and water, in the presence of hydrogen as a hydrogen source, and separating the resulting product to obtain an organic phase comprising 2,5-hexanedione; and (2) contacting the organic phase comprising 2,5-hexanedione obtained in the step (1) and ethylene with a molecular sieve catalyst for reaction to obtain paraxylene, wherein the molecular sieve catalyst is at least one selected from the group consisting of aluminophosphate molecular sieves and SCM-14 molecular sieves. The method is simple in operation, has the advantages of high product selectivity, good catalyst stability, easy product separation, few reaction steps and short time, and can realize green and efficient conversion from biomass to pX.

The invention relates to the technical field of organic synthesis, and provides a preparation method of 2, 6-bis (4-azidobenzylidene)-4-methyl cyclohexanone, which comprises the following steps: S1, carrying out aromatic nucleophilic substitution reaction on 4-nitrobenzaldehyde and azidotrimethylsilane to obtain 4-azidobenzaldehyde; and S2, carrying out an aldol condensation reaction on the 4-azidobenzaldehyde and 4-methyl cyclohexanone, so as to obtain the 2, 6-bis (4-azidobenzylidene)-4-methyl cyclohexanone. According to the technical scheme, the problems of low product yield, high cost, high energy consumption and inconvenience in large-scale industrial production of a synthetic process of 2, 6-bis (4-azidobenzylidene)-4-methyl cyclohexanone in the related technology are solved.