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221results about How to "Few reaction steps" patented technology

Polyethylene glycol-poly (2-vinyl) ethylene glycol copolymer and preparation method thereof

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.
Owner:SHAOXING XINMATE NEW MATERIALS CO LTD

Synthesis method of pyroxasulfone

The invention discloses a method for synthesizing pyroxasulfone, which comprises the following steps: by taking a raw material A and air as raw materials, carrying out oxidation reaction under the catalysis of a Fe (III) catalyst to obtain pyroxasulfone. The method has the advantages of mild reaction conditions, high yield, less three wastes, avoidance of hydrogen peroxide use and storage reactions, low cost and suitableness for industrial production.
Owner:SHANDONG RUNBO BIOTECH CO LTD

Synthesis method of toxyanib phosphate

The invention relates to the field of medicine synthesis and preparation, in particular to a synthesis method of toxyanib phosphate. The use amount of acetic acid is greatly reduced in the preparation process, so that excessive acid does not need to be neutralized in the post-treatment process, and a large amount of wastewater is not generated; in addition, the use amount of sodium nitrite is reduced, and the environment and health are facilitated; the enamine reduction reaction does not use acetic acid as a solvent and a hydrogenation reaction catalyzed by heavy metal palladium, so that the safety of the reaction is improved, and the purity of the product is also improved; a decarboxylation reaction and a Vilsmeier-Haack reaction are carried out by a one-pot method, so that the reaction steps are reduced, and the product purity is improved; when aldol reaction is carried out in side chain splicing, side reaction and generation of isomer impurities are reduced. The method is short in route, mild in reaction condition, low in equipment requirement and convenient to operate, industrial production is easy to achieve, and a complex purification method is not needed.
Owner:XIAMEN ORIGIN BIOTECH CO LTD

Method for preparing 1, 2, 3-trichloropropene with high selectivity by dehydrochlorination of 1, 2, 2, 3-tetrachloropropane

The invention discloses a method for preparing 1, 2, 3-trichloropropene with high selectivity by dehydrochlorination of 1, 2, 2, 3-tetrachloropropane, and belongs to the technical field of catalysis. The method comprises the following steps: stirring 1, 2, 2, 3-tetrachloropropane and a sodium hydroxide solution under the conditions of normal pressure and 40-100 DEG C for reflux reaction, after the reaction is finished, cooling the reaction liquid to room temperature, separating the liquid by using a separating funnel, rectifying the obtained oil phase to obtain 1, 2, 3-trichloropropene, adding an improver into the reaction system, and carrying out solid-liquid separation to obtain the 1, 2, 3-trichloropropene. The improver is a complex system composed of a metal salt and a bidentate phosphine ligand or a metal composite oxide. The method provided by the invention has the advantages of fewer reaction steps and simpler equipment, the yield of 1, 2, 3-trichloropropene is as high as 86%, the conversion rate of 1, 2, 2, 3-tetrachloropropane is as high as 92%, the selectivity of the target product is as high as 98%, and the conversion rate and the selectivity of the target product are remarkably improved.
Owner:DALIAN INSTITUTE OF CHEMICAL PHYSICS CHINESE ACADEMY OF SCIENCES

Method for improving activity of heavy magnesium oxide

The invention relates to a method for improving the activity of heavy magnesium oxide. According to the method, through the fine process steps of secondary cold water stirring, secondary time and temperature adjustment drying, primary calcination and the like, the activity of the heavy magnesium oxide is remarkably improved under the condition that the bulk density, the granularity and the crystal structure of the heavy magnesium oxide are not affected, and the active CAA value is increased from 500 seconds or above to 10 seconds to 185 seconds. In the whole preparation process, through reasonable selection of raw materials and accurate control of reaction conditions, high activity and excellent filling performance of magnesium oxide are realized, and finally, a high-performance magnesium oxide product suitable for various industrial applications is obtained. The method has the characteristics of simple process, environmental protection, high efficiency and low energy consumption, is especially suitable for large-scale production, and has wide application prospects in cobalt precipitation, sewage treatment and other industrial fields.
Owner:SHANGHAI SIIC ZHENTAI CHEM CO LTD

A method for preparing 4,4'-dihydroxybiphenyl compound

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.
Owner:SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY

Method for preparing highly branched starch by using double enzymes

PendingCN119391793Aimprove securityHigh degree of branchingFermentationCyclodextrinGlycogen branching enzyme
The invention discloses a method for preparing highly branched starch by using double enzymes, and belongs to the field of biologically modified starch. According to the invention, glycogen branching enzyme and cyclodextrin glucosyltransferase are adopted to synergistically modify different crystal forms of starch in a non-gelatinization swelling system (60 DEG C) to prepare highly branched starch, the reaction is carried out on the premise of ensuring the morphology of starch particles, and the later processing application characteristics are ensured, so that the highly branched starch can be fused with a traditional starch staple food carrier, and the preparation process is simple and convenient. According to the method, the enzyme modified starch and the swelling reaction are synchronously carried out, the step of cooling after high-temperature gelatinization is reduced, the production efficiency is improved, the adverse effect of high viscosity caused by high-temperature gelatinization on starch products is avoided, and the obtained product is high in yield, high in branching degree, low in digestibility and high in glucosidic bond proportion; a healthy and green new thought is provided for the field of starch deep processing.
Owner:JIANGNAN UNIV

Method for stereodivergently synthesizing iodo-allyl compound

The invention relates to the field of organic chemical synthesis, in particular to a method for stereodivergently synthesizing an iodo-allyl compound, which comprises an E-type iodo-allyl compound and a Z-type iodo-allyl compound. The invention provides a novel method for stereodivergently synthesizing the iodo-allyl compound, and the method is wide in substrate applicability and can be used for preparing various iodo-allyl compounds; meanwhile, in the presence of a photocatalyst or a manganese catalyst and alkali, the iodo-allyl compound can be prepared in a three-dimensional divergent manner only through visible light irradiation without high temperature and high pressure, that is, the reaction condition is mild, and the operation is simple; meanwhile, the method is wide in substrate applicability and can be used for preparing various iodo-allyl compounds. The specific initial raw materials are adopted, the initial raw materials do not need to be subjected to any other treatment and modification and can be directly used for the reaction, the reaction steps are few, the process is simple, and wide application prospects are achieved.
Owner:SOUTH CHINA UNIV OF TECH

Preparation method of oxilafluorine

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.
Owner:HAISO TECH CO LTD +1

Spiro pyrrolo-indolone derivative and preparation method thereof

The invention discloses a spiro pyrrolo-indolone derivative and a preparation method thereof, and belongs to the field of chemical synthesis, a cyclic imine ylide derivative and a 2-alkenyl indole derivative are used as raw materials, a catalyst, a solvent and alkali are added, a reaction is performed for 6-24 h, and the spiro pyrrolo-indolone derivative is obtained through one-step efficient synthesis. The preparation method has the advantages of simple operation, few reaction steps, easily available raw materials, high yield, no need of a transition metal catalyst, and environmental protection; a new path is provided for synthesizing the compounds; the enantioselectivity and diastereoselectivity of the product obtained by the preparation method disclosed by the invention are high; the preparation method has wide substrate universality and strong compatibility with substituent groups on substrates, and through one-pot one-step reaction, a tedious separation process and an intermediate compound purification process in a post-treatment process are avoided, so that time and resources are saved, and the yield is improved.
Owner:HUNAN INSTITUTE OF ENGINEERING

Method for synthesizing 3-(2-hydroperoxy-2-propyl) phenol

The invention discloses a method for synthesizing 3-(2-hydroperoxy-2-propyl) phenol and a preparation method of the 3-(2-hydroperoxy-2-propyl) phenol. The method comprises the following steps: in the presence of a solvent, 1, 3-bis (2-hydroperoxy-2-propyl) benzene is in contact with a potassium hydrogen sulfate catalyst for an acidolysis reaction, 3-(2-hydroperoxy-2-propyl) phenol is obtained, and the weight ratio of the 1, 3-bis (2-hydroperoxy-2-propyl) benzene to the catalyst is (15-48): 1. According to the method provided by the invention, 1, 3-bis (2-hydroperoxy-2-propyl) benzene (m-DHP) is used as a raw material, and a selective acidolysis reaction is carried out in the presence of a solid potassium hydrogen sulfate catalyst to obtain 3-(2-hydroperoxy-2-propyl) phenol m-HPP. The method has the characteristics of high yield, cleanness, environment friendliness, mild reaction conditions and easiness in industrialization.
Owner:CHINA PETROLEUM & CHEMICAL CORP +1

Synthesis method of pyroxasulfone

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.
Owner:HUBEI SHENGKANG CHEM CO LTD

Preparation method and application of N, N-diethyl alkyl amidine

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.
Owner:TIANJIN DAGANG OILFIELD BINGANG GRP BOHONG PETROLEUM CHEM

Novel pure organic multiple illuminant based on aryl carbazole and preparation method thereof

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 #
Owner:TIANJIN UNIV

Preparation method for rapidly synthesizing thiocyano-substituted formanilide

The invention provides a method for rapidly synthesizing thiocyano-substituted formanilide, which belongs to the technical field of organic chemical preparation, and comprises the following steps: taking alpha-aminoketone and potassium thiocyanate as initial raw materials, sealing in an oil bath pan under the condition of a copper catalyst, an oxidizing agent and an organic solvent, stirring at 80 DEG C, and heating to react for 24 hours, thereby obtaining the thiocyano-substituted formanilide. The copper catalyst comprises any one of copper chloride, copper acetate, copper sulfate, copper acetylacetonate and copper trifluoromethanesulfonate, and the oxidizing agent comprises one of iodobenzene diacetic acid, potassium persulfate, di-tert-butyl peroxide and tert-butyl hydroperoxide. The method overcomes the problems of many reaction steps, low synthesis efficiency and the like in the prior art, and has the advantages of easily available raw materials, simple operation and the like.
Owner:HUNAN INSTITUTE OF ENGINEERING

Reagents and methods for detecting monoclonal antibody drugs and anti-monoclonal antibody drug antibodies

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.
Owner:HUNAN DEMETER INSTR CO LTD

Polycaprolactone-poly (2-vinyl) ethylene glycol copolymer and preparation method thereof

PendingCN119529260AMolecular weight controllablenarrow molecular weight distributionPolymer sciencePtru catalyst
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.
Owner:SHANGHAI JIAOTONG UNIV

A method for synthesizing a tervalent tetraaryl iron porphyrin from pyrrole and aromatic aldehyde and divalent iron salt

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.
Owner:XINJIANG PUHESU NEW ENVIRONMENTAL PROTECTION MATERIAL CO LTD

Method for synergistically preparing 3, 4-dihydro-2H-benzo [b] [1, 4] thiazine from monopersulfate

The invention provides a method for synergistically preparing 3, 4-dihydro-2H-benzo [b] [1, 4] thiazine through monopersulfate, and belongs to the technical field of heterocyclic compounds. In the presence of a mixed solvent, a 2-N-benzenesulfonyl substituted phenylmethyl sulfide derivative and a halide MX are used as raw materials, and the (E)-2-(halogenated methylene)-4-p-toluenesulfonyl-3, 4-dihydro-2H-benzo [b] [1, 4] thiazine is prepared through catalysis of a catalyst monopersulfate at the reaction temperature of not more than 80 DEG C. The preparation method comprises the following steps of: preparing the (E)-2-(halogenated methylene)-4-p-toluenesulfonyl-3, 4-dihydro-2H-benzo [b] [1, 4] thiazine, the method has the advantages of simple preparation steps, mild reaction conditions, environmental protection, high product yield, high stereoselectivity, simple composition of raw materials and auxiliary materials participating in the reaction, low price, and easy obtaining, and reduces the synthesis cost.
Owner:SHAOXING UNIVERSITY +1

Method for preparing phenyl acetate with high selectivity

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.
Owner:QINGDAO UNIV OF SCI & TECH

A method for preparing a trifluoroethyl sulfide acaricide intermediate

The invention discloses a method for preparing a trifluoroethyl sulfide acaricide intermediate, wherein the method comprises: selecting cheap and readily available 2-fluoroaniline as a starting material, and preparing the intermediate through acetylation, chlorination, sulfonylation, reduction, substitution and hydrolysis, wherein the acetylation and chlorination are completed in one pot. The invention has the advantages of cheap and readily available raw materials, simple operation, short route, high yield, low cost, etc., and has certain application prospects.
Owner:ZHEJIANG UNIV OF TECH

Method for synergistically preparing 3, 4-dihydro-2H-benzo [b] [1, 4] thiazine-1-oxide from monopersulfate

The invention provides a method for synergistically preparing 3, 4-dihydro-2H-benzo [b] [1, 4] thiazine-1-oxide through monopersulfate, and belongs to the technical field of heterocyclic compounds. In the presence of an alcohol solvent, a 2-N-benzenesulfonyl substituted phenylmethyl sulfide derivative and a halide MX are used as raw materials, and the (R, E)-2-(halogenated methylene)-4-p-toluenesulfonyl-3, 4-dihydro-2H-benzo [b] [1, 4] thiazine-1-oxide with a determined spatial configuration is prepared through a catalytic reaction of a catalyst monopersulfate. The method has the advantages of simple preparation steps, mild reaction conditions, environmental protection, high product yield, high stereoselectivity, simple composition of raw materials and auxiliary materials participating in the reaction, low price, and easy obtaining, and reduces the synthesis cost.
Owner:SHAOXING UNIVERSITY +1

Preparation method of 4,1-disubstituted pyrrolo[1,2-a]quinoxaline-1-yl ketone derivatives

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.
Owner:SHIHEZI UNIVERSITY

Preparation method of 2-ethyl-6-methylaniline compound

The invention discloses a preparation method of a 2-ethyl-6-methylaniline compound, which comprises the following steps: adding a supported catalyst into a reaction device, adding 1-methoxy-2-propanol and 2-methyl-6-ethylaniline as initial raw materials, and reacting at the temperature of 60-80 DEG C for 1-2 hours to obtain the 2-ethyl-6-methylaniline compound. According to the method, 1-methoxy-2-propanol and 2-methyl-6-ethylaniline are subjected to a reaction in the absence of a solvent under the action of a supported catalyst so as to generate the 2-ethyl-6-methylaniline compound. The 2-ethyl-6-methylaniline compound is one or two of 2-ethyl-N-(2-methoxyl-1-methylethylene)-6-methylaniline and 2-ethyl-N-(2-methoxyl-1-methylethyl)-6-methylaniline, and the 2-ethyl-6-methylaniline compound is one or two of 2-ethyl-N-(2-methoxyl-1-methylethyl)-6-methylaniline and 2-ethyl-N-(2-methoxyl-1-methylethyl)-6-methylaniline. The preparation method disclosed by the invention is simple in reaction process, high in product yield and adjustable in product proportion.
Owner:ZHEJIANG UNIV OF TECH

A method for preparing olaratumab maleate

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.
Owner:SUZHOU RYAN PHARMACHEM TECH CO LTD

Berberine hydrochloride intermediate and preparation method of berberine hydrochloride

The invention relates to the technical field of organic synthesis, in particular to a berberine hydrochloride intermediate and a preparation method of berberine hydrochloride. The preparation method of the berberine hydrochloride intermediate comprises the following steps: carrying out first reaction on 2, 3-dimethoxybenzylamine and a compound A in an optional first solvent to obtain a berberine hydrochloride intermediate B; the structural formulas of the compound A and the berberine hydrochloride intermediate B are as follows: # imgabs0 #, X is selected from at least one of O, Cl and Br, and a dotted line and double lines formed by dotted lines represent single bonds or double bonds. According to the invention, the compound A and the 2, 3-dimethoxybenzylamine are subjected to mixed reaction to synthesize the key intermediate of berberine hydrochloride, so that expensive materials such as o-veratraldehyde are not used, reaction steps are reduced, and the operation is simple and convenient. The berberine hydrochloride prepared by the method is stable in quality and can be directly used for pharmaceutical production.
Owner:ZHEJIANG CAIHE BIOTECHNOLOGY CO LTD

Synthesis method of alasmigroup intermediate

The synthesis method comprises the following steps: carrying out coupling reaction on an initial raw material 1 and a compound 2 under the action of alkali and a noble metal catalyst, carrying out after-treatment, decolorizing, concentrating, dissolving and replacing to obtain a solution of a compound 3, then carrying out pressurized hydrogenation through a catalyst, and filtering out the catalyst to obtain a crude product solution of an intermediate 4, and finally, refining to obtain the ilastrant intermediate 4. According to the invention, an expensive initial material in an original research patent is replaced by 3, 4-dihydro-6-(phenylmethoxy)-1 (2H)-naphthalenone which is easier to obtain and cheaper, so that the production cost is greatly reduced; a breakthrough innovation is made on a synthesis route, tedious and lengthy synthesis steps are shortened from original seven chemical reaction steps to two chemical reaction steps, and post-treatment is simple and controllable; according to the method, the Suzuki coupling reaction catalyzed by noble metal is reduced, and the overall cost is lower on the basis of ensuring the selectivity, the stability and the high yield of the subsequent reaction.
Owner:HANGZHOU NUOAO BIOMEDICAL TECH CO LTD

A two-step synthesis method for preparing C15 alcohol for canthaxanthin

The invention discloses a two-step synthesis method of C15 alcohol for preparing canthaxanthin, wherein the synthesis method uses 4-oxo-β-ionone as a raw material, reacts with an acetylene Grignard reagent under low temperature and in an organic solvent, and hydrolyzes with a protonic acid to obtain 3-[3-hydroxy-3-methyl-penta-1-yne-4-enyl]-2,4,4-trimethyl-cyclohex-2-ene-1-one. Under a solvent, a Lindela catalyst is used for catalytic hydrogenation reaction to obtain 3-[3-hydroxy-3-methyl-penta-1,4-dienyl]-2,4,4-trimethyl-cyclohex-2-ene-1-one. The preparation method of the invention has the advantages of low raw material price, few reaction steps, mild reaction conditions, environmental friendliness, ease of operation, high reaction yield, and easy industrialization.
Owner:GUANGZHOU JUYUAN BIO-CHEM CO LTD

Alcohol hydroxyl terminated polyphenylene ether polyol and preparation method thereof

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.
Owner:DALIAN UNIV OF TECH

Photocatalytic stereoselective E-type olefination of alkynyl amide and preparation method of alkynyl amide

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.
Owner:SHAANXI UNIV OF SCI & TECH