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45results about How to "Synthetic process conditions are mild" patented technology
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Water-solubility molecule associatad three-construction units hydrophobic associated polymer and synthesizing process thereof
InactiveCN1793189AThe synthesis process conditions are simpleEase of industrial productionAlkylphenolSolubility
The invention relates to a compounding method to form water solubility intermolecular association ternary hydrophobic association polymer that includes acrylamide, sodium acrylate, and allyl-alkylphenyl aether three constructions. The method includes the following steps: using acetone as reacting solvent, alkylphenols and allyl chloride as raw material, benzyl triethyl ammonium chloride as phase-transfer catalyst, reacting for 4-8 hours at 40-60 degree centigrade to form drainage monomer allyl-alkylphenyl aether; adding sodium acrylate, acrylamide and allyl-alkylphenyl aether monomer into reactor according to the mol ratio as 20-30:69.2-79.2:0.8, adding inducing agent, sealing reacting for 2-6 hours to gain terpolymer. The terpolymer has good temperature resistance, saline tolerance, dissolubility and high temperature stability. The invention is easy to compound and has mild condition.
Owner:SICHUAN GUANGYA POLYMER CHEM
Preparation method of CoFe2O4 magnetic nano material
InactiveCN102923785AHigh saturation magnetizationSynthetic process conditions are mildMaterial nanotechnologyIron compoundsReaction temperaturePhysical chemistry
The invention provides a preparation method of a CoFe2O4 magnetic material. The preparation method comprises steps as follows: preparing a certain amount of ferric nitrate Fe(NO3)3.9H2O and a certain amount of cobalt nitrate Co(NO3)2.6H2O into a mixed solution; slowly adding to a NaOH solution with a certain concentration at a certain temperature; then agitating the reaction solution under reinforcement; maintaining the reaction temperature for a period of time; then filtering and washing until the filtrate is neutral; drying the product; grinding to obtain black brown precursors; and thermally processing the precursors for 1 hour at a certain temperature, so as to obtain the CoFe2O4 magnetic nano material.
Owner:LANZHOU UNIVERSITY OF TECHNOLOGY
Method for preparing high purity (99.9 percent) 4,4'-difluorobenzophenone
InactiveCN102531872ASynthetic process conditions are mildRecycling technology is matureCarbonyl compound preparation by condensationLiquid chlorineHydration reaction
The invention discloses a method for preparing high purity (99.9 percent) 4,4'-difluorobenzophenone, wherein 4-fluorotoluene and liquid chlorine are taken as starting raw materials and then are processed through chlorination reaction, hydration reaction and condensation reaction, and high purity (99.9 percent) 4,4'-difluorobenzophenone is obtained finally. The method gives up the conventional synthetic route; 4-fluorotoluene is processed through chlorination, hydration and condensation firstly to obtain 4,4'-difluorobenzophenone, wherein the melting point of 4,4'-difluorobenzophenone ranges from 107 to 108 DEG C, and the purity of 4,4'-difluorobenzophenone is 99.9 percent; the purity of 4,4'-difluorobenzophenone exceeds the conventional technical standard (99.7 percent) of English ICI (Imperial Chemical Industries Ltd.); in the preparation technology of the method, the adopted raw materials are easy to get, the synthesis process conditions are mild, and almost no environment hazards can be caused. The method satisfies the technical requirements of special engineering plastic containing polyether-ether-ketone on monomers.
Owner:JINTAN CHUNFENG CHEM
Preparation method of polyaniline@polypyrrole conductive composite material
InactiveCN102964831AImprove conductivity stabilityImprove conductivityPolypyrroleIn situ polymerization
The invention discloses a preparation method of a polyaniline@polypyrrole conductive composite material, which comprises the following steps of: firstly synthesizing PAn by a chemical oxidation method, and performing leaching, cleaning and drying to obtain deep green powder of PAn; then mixing a certain amount of polyaniline with a certain amount of water by an in-situ polymerization method, adding doping agent sulfamic acid and pyrrole monomer respectively, uniformly stirring the mixed liquid, and adding an oxidant ferric trichloride; then filtering the reaction liquid, and washing until the filtrate is neutral; and finally drying the filter cake and grinding to obtain black polyaniline@polypyrrole conductive powder.
Owner:LANZHOU UNIVERSITY OF TECHNOLOGY
Imine salt derivative, preparation method thereof and preparation method of nicotine
InactiveCN110627769ASynthetic process conditions are mildMeet growth requirementsOrganic compound preparationGroup 5/15 element organic compoundsNicotine synthesisSolvent
The invention discloses an imine salt derivative, a preparation method thereof and a preparation method of nicotine. The preparation method of nicotine includes the steps of: adding an imine salt derivative shown as general formula (I) or (II) in the specification and a reducing agent into a solvent for reaction to prepare a racemic nicotine solution; adding a second quenching agent into the racemic nicotine solution to obtain a nicotine precursor solution; and adding an extracting agent into the nicotine precursor solution, conducting reduced pressure concentration, and performing drying andremoving the solvent, thus obtaining nicotine. According to the invention, through the imine salt derivative intermediate synthesized for the first time and the use of the cheap reducing agent, the intermediate is reduced under a relatively mild condition to obtain racemic nicotine. Compared with the existing nicotine synthesis process, the method has the advantages of mild synthesis process conditions, simple equipment requirement, high product purity and high synthesis rate, and is particularly suitable for industrial production.
Owner:SHENZHEN HELGETECH CO LTD
Method for preparing high-purity 4,4'-difluorobenzophenone
ActiveCN104610035ARaw materials are cheap and easy to getSynthetic process conditions are mildOrganic compound preparationCarbonyl compound preparation by condensationEnvironmental resistancePolyether ether ketone
The invention discloses a method for preparing high-purity 4,4'-difluorobenzophenone. p-fluorotoluene is used as an initial raw material and oxidation reaction, chloroformylation reaction and condensation reaction are carried out, so that the target product 4,4'-difluorobenzophenone is finally obtained; the melting point of the product is 107-109 DEG C; the purity of the product is greater than or equal to 99.9 percent and accords with the purity requirement for synthesis of polyether-ether-ketone (PEEK). Moreover, according to the preparation method disclosed by the invention, the used raw material is cheap and is easy to obtain, the synthetic process conditions are mild and in the synthesizing process, a used reagent is relatively green and environmental-friendly, and thus, the method has wide application prospect and high industrial value.
Owner:RUYUAN YAO AUTONOMOUS COUNTY DONGYANGGUANG FORMED FOIL CO LTD
Method for efficient catalytic synthesis of epoxy bisphenol fluorene
InactiveCN111574482AReduce pollutionThe synthesis steps are simpleOrganic chemistryPtru catalystDistillation
The invention relates to the technical field of chemical engineering chemistry, in particular to a method for efficient catalytic synthesis of epoxy bisphenol fluorene. The method can effectively shorten the reaction time, simplify the reaction steps, conveniently control the reaction temperature and effectively improve the product yield, and the product is easy to purify and good in chromaticity.The method comprises the following steps: S1, mixing and dissolving; S2, catalytic reaction: adding a catalyst into the reaction solution obtained in the step S1, adjusting the temperature of the reaction solution to 50-100 DEG C, and reacting for 3-6 hours; S3, adding alkali for reaction: adjusting the temperature of the reaction solution to 30-70 DEG C, adding alkali into the reaction solution,adjusting the temperature of the reaction solution to 50-80 DEG C, and continuing to react for 1-3 hours; S4, filtering and separating; S5, water washing treatment; S6, distillation treatment; S7, recrystallization: adding a recrystallization solvent into the white solid product obtained in the step S6, fully dissolving to obtain a recrystallization mixed solution, lowering the temperature of themixed solution to-5 DEG C, and cooling to separate out; S8, performing centrifugal separation; and S9, performing drying treatment.
Owner:HUANGHUA XINNUOLIXING FINE CHEM
New method for synthesizing dietary supplement melatonin
ActiveCN113402437AThe synthesis process is simpleSynthetic process conditions are mildOrganic chemistryFood ingredient functionsChemical synthesisSerotonin
The invention discloses a novel method for synthesizing a dietary supplement melatonin, and belongs to the technical field of pharmaceutical chemical synthesis. According to the method, N-acetyl serotonin is used as a starting raw material, melatonin is obtained through one-step methylation reaction, the synthesis process is simple, the synthesis process conditions are mild, the yield is as high as 98.5% or above, the quality is good, the content is larger than 99.5%, and the melatonin completely meets the USP42 standard. The new method for synthesizing the dietary supplement melatonin provided by the invention saves the cost and is easy for industrial production.
Owner:河北维达康生物科技有限公司
Pd composite nano-catalyst for hydrogen production by formic acid decomposition and preparation method of Pd composite nano-catalyst
ActiveCN110026236AHigh activitySynthetic process conditions are mildHydrogenOrganic-compounds/hydrides/coordination-complexes catalystsNano catalystDecomposition
The invention discloses a Pd nano-composite catalyst for catalyzing formic acid decomposition to produce hydrogen and a preparation method of the Pd nano-composite catalyst, and belongs to the field of hydrogen storage materials. The catalyst is prepared by loading ultra-small Pd nanoclusters on the surface of a composite carrier composed of an inorganic carrier and amino-modified graphene oxide.The preparation method comprises the following steps: compounding graphene oxide and an inorganic nano material under the action of chemical bonds through long-time stirring; conducting amino modification on the outer surface of the graphene oxide, then adding a salt solution of Pd, and conducting sodium borohydride reduction to enable monodisperse Pd nano-clusters to be stabilized on the surfaceof the carrier, so as to obtain the Pd nano-composite catalyst which can be used for efficiently catalyzing decomposition of formic acid to produce hydrogen. The synthesis process provided by the invention is mild in condition, the catalyst has very high activity in catalyzing of formic acid decomposition to produce hydrogen under mild conditions, is easy to separate from a system after catalysisis finished, can be recycled, can be prepared on a large scale, is applicable to practical application, and has a wide application prospect in the fields of chemical hydrogen storage materials, fuel cells and the like.
Owner:DALIAN UNIV OF TECH
Efavirenz intermediate synthesizing method
InactiveCN106946718AEasy to recycleLow costOrganic compound preparationOrganic chemistry methodsDistillationAniline
The invention relates to an efavirenz intermediate synthesizing method. The efavirenz intermediate synthesizing method comprises the following steps of: adding cyclopropyl acetylene magnesium bromide to a coordination compound prepared from neopentyl alcohol, a zinc salt or copper salt and (1R, 2S)-1-phenyl-2-(1-pyrrolidyl)-1-propyl alcohol by using 2-methyltetrahydrofuran as a solvent, reacting, adding 4-chlorine-2-(trifluoroacetyl) aniline, and carrying out heat-preservation stirring till ending; and transferring to a saturated citric acid solution for quenching, carrying out reduced pressure distillation after separating to obtain an organic phase, adding an polar organic solvent and L-amino acid after obtaining racemate, heating and mixing, carrying out cooling crystallization after resolution, and carrying out recrystallization after obtaining crystals to obtain white powder. Compared with the prior art, the efavirenz intermediate synthesizing method has the advantages that the 2-methyltetrahydrofuran which is a green solvent is used in reaction; the product with relatively high optical purity is obtained by using very few organic ligands; the yield is relatively high; the selectivity is good; the separation of products and the control of reaction conditions are easy; and the method conforms to green and environmental protection concept and is suitable for industrialized production.
Owner:WUHAN INSTITUTE OF TECHNOLOGY
Calix[4]thiourea diaminocyclohexane derivatives and method thereof for catalyzing asymmetric Michael addition
InactiveCN108727241AEffective Phase Transfer CatalysisSynthetic process conditions are mildOrganic chemistryOrganic compound preparationChromatographic separationNitroalkene
The invention relates to calix[4]thiourea diaminocyclohexane derivatives and a method thereof for catalyzing asymmetric Michael addition. An Michael addition catalytic reaction is performed on nitroolefin and 1,3-dicarbonyl ketone as raw materials, the calix[4]thiourea diaminocyclohexane derivatives as a phase transfer catalyst and water / toluene as a solvent, after the reaction, the solvent is concentrated, and a product is obtained by column chromatographic separation on silica gel. The calix[4]thiourea diaminocyclohexane derivatives adopt mild synthesis process conditions and are high in catalysis efficiency, water / toluene is taken as the solvent for asymmetric Michael addition catalyzed by the derivatives, reaction speed and yield can be increased greatly by water addition, and the catalyst has a phase transfer catalysis function. Better ee value can be obtained by the catalytic reaction at room temperature, and the derivatives have broad application prospect.
![Calix[4]thiourea diaminocyclohexane derivatives and method thereof for catalyzing asymmetric Michael addition](https://images-eureka.patsnap.com/patent_img/7c46d7ac-c168-4c43-b645-f55ee7583e0b/BDA0001668876310000021.png "Calix[4]thiourea diaminocyclohexane derivatives and method thereof for catalyzing asymmetric Michael addition")
![Calix[4]thiourea diaminocyclohexane derivatives and method thereof for catalyzing asymmetric Michael addition](https://images-eureka.patsnap.com/patent_img/7c46d7ac-c168-4c43-b645-f55ee7583e0b/BDA0001668876310000041.png "Calix[4]thiourea diaminocyclohexane derivatives and method thereof for catalyzing asymmetric Michael addition")
![Calix[4]thiourea diaminocyclohexane derivatives and method thereof for catalyzing asymmetric Michael addition](https://images-eureka.patsnap.com/patent_img/7c46d7ac-c168-4c43-b645-f55ee7583e0b/BDA0001668876310000071.png "Calix[4]thiourea diaminocyclohexane derivatives and method thereof for catalyzing asymmetric Michael addition")
Owner:CHANGZHOU UNIV
Method for preparing pH-responsive comb-structure polycarboxylic acid through terminal group functionalization
The invention relates to a method for preparing pH-responsive comb-structure polycarboxylic acid through terminal group functionalization. According to the method, with a pH-responsive monomer, unsaturated halogenated hydrocarbon, a small carboxylic acid momonomer and the like as raw materials, a polycarboxylate material is prepared through self-polymerization first, then substitution and then copolymerization; namely, with the pH-responsive monomer as a reactant, a terminal group-functionalized pH-responsive polymer chain is produced through the self-polymerization under the actions of an initiator and a terminal group functionalizing agent, then a substitution reaction is performed on the terminal group-functionalized pH-responsive polymer chain and the unsaturated halogenated hydrocarbon to obtain a pH-responsive macromonomer, and finally a copolymerization reaction is performed on the pH-responsive macromonomer and the small carboxylic acid momonomer under the action of the initiator to obtain a comb-structure polymer which uses polycarboxylic acid as a main chain and has a side chain with a pH-responsive function. By the method, the process is high-efficiency and energy-saving, the conversion rate of a product is high, the functional modification of the polycarboxylic acid is successfully achieved through introduction of the pH-responsive polymer side chain by a terminal group functionalization method, an excellent characteristic of inhibiting shrinkage of cement mortar is shown, and the market competitiveness and the application prospect are very good.
Owner:BEIJING UNIV OF TECH
Preparation method of polypyrrole/organically modified attapulgite conductive composite material
The preparation method of polypyrrole / organic modified attapulgite conductive composite material, first mix a certain amount of attapulgite, a certain amount of organic modifier and a certain amount of water, stir and react for a certain period of time, and then filter the filter cake Drying, crushing to obtain organically modified attapulgite; then mixing a certain amount of organically modified attapulgite with a certain amount of water, and then adding dopant sulfamic acid and pyrrole monomer respectively, and stirring the mixture evenly , add the oxidant ferric chloride, react for a certain period of time and then add a certain amount of HCl solution for secondary doping, then filter the reaction solution and wash until the filtrate is neutral; finally dry the filter cake and pulverize it to obtain polypyrrole / concave-convex Stick clay black conductive powder.
Owner:LANZHOU UNIVERSITY OF TECHNOLOGY
Polyaniline corrosion inhibitor and preparation method thereof
ActiveCN110591355ASimple manufacturing processSynthetic process conditions are mildCelluloseOrganic acid
The invention relates to an organic polymer corrosion inhibitor, in particular to a polyaniline corrosion inhibitor and a preparation method thereof. The corrosion inhibitor comprises the following raw materials: hydroxypropyl methylcellulose, ammonium persulfate, aniline and water; and the molar ratio of the hydroxypropyl methylcellulose, the ammonium persulfate and the aniline is 1: (2.84-4.32):(2.97-8.92). The preparation method comprises the following steps: firstly, mixing the hydroxypropyl methylcellulose with the water to form a hydroxypropyl methylcellulose solution, and then dropwiseadding an ammonium persulfate solution into the hydroxypropyl methylcellulose solution for oxidation reaction; and finally, dropwise adding an aniline solution into the reaction solution at a low temperature to carry out polymerization reaction, washing a filter cake by an organic solvent after the reaction is finished, and drying the filter cake to obtain cellulose-doped polyaniline. The polyaniline corrosion inhibitor has the advantages of simple manufacturing process flow, mild synthesis process conditions and no addition of other organic acids or inorganic acids; and the used raw materialcellulose is wide in source, harmless and nontoxic, the aniline raw material is easy to obtain, and the synthesized cellulose-doped polyaniline can be used for sustained-release protection on metalsin an acid solution.
Owner:LANZHOU UNIVERSITY OF TECHNOLOGY
Synthesis method of zirconocene olefin polymerization catalyst
PendingCN114507305ARealize industrial productionSynthetic process conditions are mildMetallocenesCyclopentenePolymer science
The invention relates to a synthesis method of a zirconocene olefin polymerization catalyst, belonging to the technical field of synthesis of organic and high polymer materials. The preparation method comprises the following steps: reacting 3-bromothiophene with strong base, and carrying out methylation reaction with methyl iodide to obtain 2-methyl-3-bromothiophene; the preparation method comprises the following steps: carrying out a Friedel-Crafts acylation reaction, a Nashroff cyclization reaction and a Suzuki coupling reaction on 2, 5-dimethyl-3-phenyl-5, 6-dihydrocyclopentane [1, 2-b] thiophene-4-ketone to obtain 2, 5-dimethyl-3-phenyl-5, 6-dihydrocyclopentane [1, 2-b] thiophene-4-ketone; carrying out reduction and elimination to obtain 2, 5-dimethyl-3-phenyl-6-cyclopentene [1, 2-b] thiophene; and finally, carrying out silylation and zircon salt coordination to obtain the target zirconocene type olefin polymerization catalyst. The synthesis conditions are relatively mild, the synthesis method is low in cost and low in energy consumption, and industrial production of the catalyst is facilitated.
Owner:JILIN UNIV
A kind of PD composite nano-catalyst and preparation method thereof for formic acid decomposition hydrogen production
ActiveCN110026236BHigh activitySynthetic process conditions are mildHydrogenOrganic-compounds/hydrides/coordination-complexes catalystsNano catalystPtru catalyst
The invention discloses a Pd nanocomposite catalyst for catalyzing the decomposition of formic acid to produce hydrogen and a preparation method thereof, belonging to the field of hydrogen storage materials. The catalyst is prepared by loading ultra-small Pd nano-clusters on the surface of a composite support composed of an inorganic support and amino-modified graphene oxide. The preparation method comprises: compounding graphene oxide and inorganic nanomaterials under the action of chemical bonds by stirring for a long time, and then modifying the outer surface of graphene oxide with amino groups, then adding a Pd salt solution, and reducing the graphene oxide by sodium borohydride. The dispersed Pd nanoclusters are stabilized on the surface of the carrier, and the obtained Pd nanocomposite catalyst can be used to efficiently catalyze the decomposition of formic acid to produce hydrogen. The synthesis process of the present invention has mild conditions, and has very high activity in catalyzing the decomposition of formic acid to produce hydrogen under mild conditions. After the catalysis is completed, it is easy to separate from the system and can be recycled. And fuel cells and other fields have broad application prospects.
Owner:DALIAN UNIV OF TECH
Stable isotope labelled sulfamethazine and synthesis method thereof
ActiveCN110028457ASynthetic process conditions are mildSimple processIsotope introduction to heterocyclic compoundsSulfonyl chlorideStable Isotope Labeling
The invention discloses stable isotope labelled sulfamethazine and a synthesis method thereof. The synthesis method comprises the following steps: S1: enabling stable isotope labelled aniline and acetic anhydride to react to prepare stable isotope labelled acetyl aminobenzene; S2: enabling the stable isotope labelled acetyl aminobenzene to react with chlorosulfonic acid to obtain stable isotope labelled p-acetamidobenzene sulfonyl chloride; S3: enabling the stable isotope labelled p-acetamidobenzene sulfonyl chloride to react with 2-amino-4,6-dimethyl-5-bromine pyrimidine, hydrolyzing the formed intermediate under the alkaline condition, and obtaining the stable isotope labelled sulfamethazine. Compared with the prior art, the condition of the synthesis process is mild, the process is simple, the process route is short, a product is easy to separate and purify, the yield is high, the chemical purity and the abundance of the stable isotope of the obtained product are both 99% or higherand meet the requirements of a standard reagent used for quantitatively detecting sulfabromomethazine; the use value is high, and the economic efficiency of the stable isotope labelled sulfamethazineis excellent.
Owner:FOOD INSPECTION CENT OF CIQ SHENZHEN +1
Method for preparing concrete water reducer with styrene sulfonate as monomers
The invention discloses a method for preparing a concrete water reducer with styrene sulfonate as monomers, and belongs to the field of water reducers. The method includes the steps that firstly, styrene sulfonate and unsaturated carboxylic acid monomers are subjected to free radical copolymerization to obtain a polycarboxylic acid-styrene sulfonate main chain, and then benzene sulfonate on the main chain is modified into phenylsulfonyl halide groups; then, an oxidation-reduction initiating system is formed by high-valence cerate and alcohol to initiate polymerization of unsaturated cationic quaternary ammonium monomers to obtain a hydroxyl-terminated cationic long chain; then, the polycarboxylic acid main chain containing the phenylsulfonyl halide groups, the hydroxyl-terminated cationic long chain and a polyethylene glycol compound are subjected to sulfonylation to obtain the concrete water reducer. According to the method, based on the molecular structure design principle, by modifying styrene sulfonate into phenylsulfonyl halide and carrying out sulfonylation on grafted cationic side chains and polyethylene glycol side chains, the novel concrete water reducer containing a double-side-chain structure is successfully synthesized; the reaction process is mild, easy to control, capable of saving energy and efficient, and the concrete water reducer shows multiple excellent effects of water reduction for slump loss resistance, clay resistance and the like.
Owner:BEIJING UNIV OF TECH
Preparation method of efavirenz intermediate
InactiveCN106986781ANot easy to absorb waterNot easy to saveOrganic compound preparationAmino-hyroxy compound preparationEnvironmental resistanceOil phase
The invention relates to a preparation method of an efavirenz intermediate. The method comprises the following steps of reacting a zinc salt or copper salt with an organic ligand (1R, 2S)-1-phenyl-2-(1-pyrrolidyl)-1-propyl alcohol in an organic solvent, adding a cyclopropylene reagent; stirring at a constant temperature for 2h and adding 1-(5-chloro-2-nitrophenyl)-2,2,2-trifluoro-ethanone, completing stirring reaction, adding a proton source for quenching reaction and separating an organic phase from an aqueous phase through extraction; and adding an oil phase which is obtained through direct concentration and drying of the organic phase to a solution of tetrahydrofuran and methyl alcohol at a certain ratio, and then adding acetic acid and iron powder, stirring and filtering the obtained mixture through kieselguhr, washing, drying, carrying out vacuum concentration and purifying to obtain an efavirenz key intermediate. The 1-(5-chloro-2-nitrophenyl)-2,2,2-trifluoro-ethanone is utilized for participating in reaction, so that the method is short in process, mild in condition, simple in operation, green, environment-friendly and low in cost.
Owner:WUHAN INSTITUTE OF TECHNOLOGY
Saturated polyester type low-shrinkage additive and application thereof
The invention discloses a saturated polyester type low-shrinkage additive which is prepared by the following steps: mixing polyhydric alcohols with three or more degrees of functionality with a lactone monomer, and heating to 140-170 DEG C under the protection of nitrogen; dropwise adding a catalyst, and carrying out a reflux reaction for 5-8 h at a temperature of 150-155 DEG C after the dropwiseaddition is completed; cooling to 90-100 DEG C, adding a polymerization inhibitor, uniformly stirring, adding an active diluent for dilution after the polymerization inhibitor is completely dissolved,cooling and filtering to obtain the saturated polyester type low-shrinkage additive. The saturated polyester low shrinkage agent has an excellent shrinkage rate control effect, and can make the coloring property of BMC better.
Owner:广东百汇达新材料有限公司
Calix[4]squaramide cyclohexanediamine derivative and method for catalyzing asymmetric Michael addition and acetalization tandem reaction by using derivative
ActiveCN110283087ASynthetic process conditions are mildHigh catalytic efficiencyOrganic compound preparationOrganic-compounds/hydrides/coordination-complexes catalystsUnsaturated ketoneChemistry
The invention belongs to the technical field of catalytic organic synthesis, and specifically relates to a calix[4]squaramide cyclohexanediamine derivative and a method for catalyzing an asymmetric Michael addition and acetalization tandem reaction by using the derivative. With an unsaturated keto ester and 1,3-dicarbonyl cycloketone as raw materials, the calix[4]squaramide cyclohexanediamine derivative as a catalyst, and dichloromethane as solvent, the Michael addition and acetalization tandem catalytic reaction is performed; after the reaction is finished, the solvent is concentrated and a product is obtained through separation by silica gel column chromatography. A calix[4]squaramide cyclohexanediamine catalyst involved in the invention is mild in synthesis process conditions, the separation of an intermediate is not needed, the catalytic efficiency is high, a relatively good ee value can be obtained by the catalytic reaction under the condition of room temperature, and broad application prospects are realized.
![Calix[4]squaramide cyclohexanediamine derivative and method for catalyzing asymmetric Michael addition and acetalization tandem reaction by using derivative](https://images-eureka.patsnap.com/patent_img/18584a59-1675-4f31-83de-6d8580b0889b/HDA0002141679010000011.png "Calix[4]squaramide cyclohexanediamine derivative and method for catalyzing asymmetric Michael addition and acetalization tandem reaction by using derivative")
![Calix[4]squaramide cyclohexanediamine derivative and method for catalyzing asymmetric Michael addition and acetalization tandem reaction by using derivative](https://images-eureka.patsnap.com/patent_img/18584a59-1675-4f31-83de-6d8580b0889b/FDA0002141674990000011.png "Calix[4]squaramide cyclohexanediamine derivative and method for catalyzing asymmetric Michael addition and acetalization tandem reaction by using derivative")
![Calix[4]squaramide cyclohexanediamine derivative and method for catalyzing asymmetric Michael addition and acetalization tandem reaction by using derivative](https://images-eureka.patsnap.com/patent_img/18584a59-1675-4f31-83de-6d8580b0889b/BDA0002141675000000021.png "Calix[4]squaramide cyclohexanediamine derivative and method for catalyzing asymmetric Michael addition and acetalization tandem reaction by using derivative")
Owner:CHANGZHOU UNIV
Method for preparing concrete water reducing agent with p-styrene sulfonate as monomer
Owner:BEIJING UNIV OF TECH
Stable isotope labeled metronidazole and synthesis method thereof
PendingCN114075142ASynthetic process conditions are mildSimple processIsotope introduction to heterocyclic compoundsNitroimidazoleStable Isotope Labeling
The invention discloses stable isotope labeled metronidazole and a synthesis method thereof. The synthesis method comprises the following steps: S1, carrying out intramolecular ring closing on stable isotope labeled bromoethanol under an alkaline condition to prepare stable isotope labeled ethylene oxide; and S2, reacting the stable isotope labeled ethylene oxide and 2-methyl-5-nitroimidazole, to obtain the stable isotope labeled metronidazole. Compared with the prior art, the synthetic process is mild in condition, simple in process and short in process route, the product is easy to separate and purify, the chemical purity and stable isotope abundance of the obtained product both reach 99% or above, and the requirements of the product as a standard reagent for quantitative detection of metronidazole are met; and the use value is high, and the economical efficiency is good.
Owner:SHANGHAI ANPEL SCI INSTR
Synthesis method of stable isotope labeled 3-chloro-1,2-propylene glycol fatty acid diester
ActiveCN112899315ASynthetic process conditions are mildSimple processOrganic compound preparationFermentationStable Isotope LabelingFatty acid
The invention discloses a synthesis method of stable isotope labeled 3-chloro-1,2-propylene glycol fatty acid diester. The synthesis method comprises the following steps: S1, hydrolyzing stable isotope labeled epoxy chloropropane to prepare stable isotope labeled 3-chloro-1,2-propylene glycol; and S2, carrying out a reaction on the stable isotope labeled 3-chloro-1,2-propylene glycol and fatty acid acyl chloride under the catalytic action of the immobilized lipase to prepare the 3-chloro-1,2-propylene glycol fatty acid diester. The synthesis process has characteristics of mild conditions, simple process, short process route, easy product separation and purification and high yield, the chemical purity and the stable isotope abundance of the obtained product achieve more than 99% so as to meet the requirements of the standard reagent for quantitative detection of 3-chloro-1,2-propylene glycol fatty acid diester; and the use value is high, and the economical efficiency is good.
Owner:上海安谱璀世标准技术服务有限公司
Preparation method of multifunctional asphalt stripping agent
The invention discloses a preparation method of a multifunctional asphalt stripping agent. The preparation method comprises following steps: under nitrogen gas protection, with stirring, a mixed solution of methyl acrylate and methanol is added into an organic polyamine solution dropwise, after dropwise adding, an obtained mixture is stirred for reaction at room temperature so as to obtain a transparent light yellow liquid intermediate; the transparent light yellow liquid intermediate is subjected to distillation to remove methanol, and is subjected to heating condensation polymerization to remove impurities so as to obtain a yellow thick liquid NH2-HBP; alkali lignin is prepared into an aqueous solution A; the NH2-HBP product is prepared into an aqueous solution B; an initiator is added for mixing stirring, reaction is carried out at 60 to 80 DEG C, and deposition, washing, and drying are carried out so as to obtain the multifunctional asphalt stripping agent. The multifunctional asphalt stripping agent possesses excellent stripping performance, anti-ultraviolet performance, and antioxidation performance, and is low in raw material cost and viscosity, excellent in intermiscibilitywith asphalt, and relatively mild in synthesis technology conditions.
Owner:盘锦辽河油田大力集团有限公司
Preparation method and application of a nitrogen-doped carbon material catalyst
ActiveCN109248700BLow costShort preparation cyclePhysical/chemical process catalystsCarboxylic acid nitrile preparationPtru catalystHydrogen selectivity
The invention provides a method for preparing a nitrogen-doped carbon material catalyst, comprising the following steps: A, adding a nitrogen-containing compound and a carbon material into ethanol respectively, and stirring for 5-20 hours at a temperature range of 0-70°C; B. 1. Separating the liquid obtained in step A into solid-liquid, and drying the separated solid; C. Grinding the dried solid obtained in step B, and calcining it under an inert atmosphere to obtain a nitrogen-doped carbon material catalyst. The catalyst described in the invention can efficiently and selectively catalyze the hydrogenation of aromatic compounds under mild conditions, reduce the amount of metal used, reduce the cost of the catalyst, improve catalyst activity, stability and hydrogenation selectivity, and also have good electrocatalytic performance .
Owner:TIANJIN UNIV
Synthesizing method of sitagliptin key intermediate
ActiveCN105254519AHigh optical puritySynthetic process conditions are mildOrganic compound preparationAmino-carboxyl compound preparationBenzeneHelium atom
The invention relates to the technical field of medicine, in particular to a synthesizing method of a sitagliptin key intermediate. The sitagliptin key intermediate (R)-4-chloro-3-amino-4-(2,4,5-trifluoro-phenyl)butyrate after the raw material trifluoro-benzene is subjected to friedel-crafts acylation, hydrolysis, helium atom replacement, condensation, ammonolysis, hydrogenation reduction and hydrolysis. The method has the advantages that low-price trifluoro-benzene serves as the initial raw material and is wide in source; the chiral center is established through a hydrogenation reduction in which metal rhodium and chiral ferrocenyl diphosphine participate, helium atoms are introduced to the left side of a reaction locus, and therefore the optical purity of the product is effectively improved; the synthesis process conditions are mild and easy to control.
Owner:GENCHEM & GENPHARM CHANGZHOU CO LTD
A method for preparing high-purity 4,4'-difluorobenzophenone
ActiveCN104610035BMeet purity requirementsRaw materials are cheap and easy to getOrganic compound preparationCarbonyl compound preparation by condensationBenzophenonePolyether ether ketone
The invention discloses a method for preparing high-purity 4,4'-difluorobenzophenone. p-fluorotoluene is used as an initial raw material and oxidation reaction, chloroformylation reaction and condensation reaction are carried out, so that the target product 4,4'-difluorobenzophenone is finally obtained; the melting point of the product is 107-109 DEG C; the purity of the product is greater than or equal to 99.9 percent and accords with the purity requirement for synthesis of polyether-ether-ketone (PEEK). Moreover, according to the preparation method disclosed by the invention, the used raw material is cheap and is easy to obtain, the synthetic process conditions are mild and in the synthesizing process, a used reagent is relatively green and environmental-friendly, and thus, the method has wide application prospect and high industrial value.
Owner:RUYUAN YAO AUTONOMOUS COUNTY DONGYANGGUANG FORMED FOIL CO LTD
Method for preparing optical activity 2,3-dihydroxy teinai hemiacetal derivant
InactiveCN101130529BHigh optical puritySynthetic process conditions are mildAsymmetric synthesesButanediolBenzyl group
The invention discloses a making method of 2, 3-dihydroxy butyl inner hemiacetal derivative with optical activity as chiral intermediate, which comprises the following steps: preparing tartrate ester (3); making tartrate ester (4) protected by alkyl or benzyl or silicon as R1; making 1, 4-butanediol (5); making 2,3-dihydroxy dihydroxy butyl inner hemiacetal derivative (1) under mild synthesizing technique and easy operation with high receiving rate. The invention improves the optical purity of the product, which is a convenient, economic and high-effective product.
Owner:XIAMEN UNIV
Method for preparing ph-responsive comb-like structure polycarboxylic acid by end group functionalization
The invention relates to a method for preparing pH-responsive comb-structure polycarboxylic acid through terminal group functionalization. According to the method, with a pH-responsive monomer, unsaturated halogenated hydrocarbon, a small carboxylic acid momonomer and the like as raw materials, a polycarboxylate material is prepared through self-polymerization first, then substitution and then copolymerization; namely, with the pH-responsive monomer as a reactant, a terminal group-functionalized pH-responsive polymer chain is produced through the self-polymerization under the actions of an initiator and a terminal group functionalizing agent, then a substitution reaction is performed on the terminal group-functionalized pH-responsive polymer chain and the unsaturated halogenated hydrocarbon to obtain a pH-responsive macromonomer, and finally a copolymerization reaction is performed on the pH-responsive macromonomer and the small carboxylic acid momonomer under the action of the initiator to obtain a comb-structure polymer which uses polycarboxylic acid as a main chain and has a side chain with a pH-responsive function. By the method, the process is high-efficiency and energy-saving, the conversion rate of a product is high, the functional modification of the polycarboxylic acid is successfully achieved through introduction of the pH-responsive polymer side chain by a terminal group functionalization method, an excellent characteristic of inhibiting shrinkage of cement mortar is shown, and the market competitiveness and the application prospect are very good.
Owner:BEIJING UNIV OF TECH
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