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Compound for preparing suvorexant and preparation method thereof
ActiveCN103923068AAvoid chiral separation and the use of chiral catalystsEasy to operateCarbamic acid derivatives preparationOrganic compound preparationStereochemistryStereoisomerism
The invention relates to three novel compound formulas I, II and III for preparing suvorexant, stereoisomers or salt thereof and a preparation method of the formulas I, II and III. The invention also relates to a method for preparing the suvorexant. The preparation method disclosed by the invention can be used for synthesizing to obtain the chiral compounds I, II and III through a chiral initiator and use the chiral compounds I, II and III for the synthesis of the suvorexant and has the advantages of easiness for operation, moderation in reaction condition, easiness for post processing, easiness for purification, high yield, high ee value and easiness for industrialization.
Owner:武汉久安药业有限公司
Method for rapidly producing biodiesel from kitchen garbage and produced biodiesel
InactiveCN103242914AShort reaction timeMild reaction conditionsFatty oils/acids recovery from wasteFatty acid chemical modificationBiodieselMass ratio
The invention provides a method for rapidly producing biodiesel from kitchen garbage and produced biodiesel. The method comprises the following steps of: (1) carrying out pretreatment: enabling the kitchen garbage to be subjected to sorting, crushing and vacuum dewatering, thereby obtaining hogwash oil; (2) weighing methanol and the hogwash oil in accordance with that the mass ratio of the methanol to the hogwash oil is (50: 100) to (500: 100), and weighing a catalyst in accordance with that the catalyst accounts for 0.05-5% by mass of the oil; (3) dissolving the catalyst in the methanol, and adding the hogwash oil and the methanol where the catalyst is dissolved to an autoclave for reacting for 3-60 min at the temperature of 80-350 DEG C and the pressure of 1-10 MPa; and (4) after the reaction is completed, carrying out reduced-pressure distillation, recovering excessive methanol, and enabling a product to be subjected to standing for layering, wherein a lower layer is glycerine, and an upper layer is the biodiesel. The method provided by the invention has the characteristics of short reaction time, mild reaction conditions and simple product post-processing.
Owner:GUANGZHOU SPECIAL PRESSURE EQUIP INSPECTION & RES INST
NNN ligand, metal complexes thereof, preparation methods and application
ActiveCN105294667AHigh yieldMild reaction conditionsCobalt organic compoundsIron organic compoundsRegioselectivityAlkene
The invention discloses an NNN ligand, metal complexes thereof, preparation methods and application, and particularly provides an NNN ligand 1, a metal complex 2 of the NNN ligand, a metal complex 3 of the NNN ligand and preparation methods of the NNN ligand 1 and the metal complexes, as well as application of the metal complex 3 of the NNN ligand to catalysis on hydroboration reaction of bis-substituted olefin, especially application of the metal complex 3 to catalysis on asymmetric hydroboration reaction of 1, 1-bis-substituted olefin. The metal complex 3 of the NNN ligand has good catalytic activity in the hydroboration reaction of the bis-substituted olefin, especially asymmetric hydroboration reaction of the 1, 1-bis-substituted olefin, has excellent regioselectivity and enantioselectivity, and is high in yield and mild in reaction conditions; besides, the preparation methods of the NNN ligand and the metal complexes thereof are simple, environment-friendly, mild in reaction conditions, relatively high in yield, and simple in post-processing, and the raw materials are low in cost and easy to obtain, so that the preparation methods are suitable for industrial production. (The formulas of the NNN ligand 1, metal complex 2 and metal complex 3 are shown in the description).
Owner:SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
Synthesizing method for amide compound
ActiveCN104710259ADiversity is cheap and readily availableReduce manufacturing costOrganic compound preparationCarboxylic acid amides preparationAir atmosphereAlcohol
The invention discloses a synthesizing method for an amide compound shown in formula (III). The synthesizing method comprises the following steps: adopting replacing acetonitrile shown in formula (I) and amines compound shown in formula (II) as raw materials in air atmosphere; adopting Ru / C as a catalyst; conducting reaction in solvent to generate the amide compound shown in formula (III); the solvent is one selected from ethyl alcohol, furanidine, methyl sulfoxide and o-dichlorobenzene. The synthesizing method being novel synthesizing route is simple to operate, convenient in post-treatment, high in product yield, and good in product purity; particularly, the catalyst and the solvent can be used repeatedly; air is taken as oxidant; not only production cost is reduced, but also the method is environmental-friendly, and very suitable for large-scale industrialization production.
Owner:ZHEJIANG UNIV OF TECH
Method for synthesizing alpha-pyranone derivatives
InactiveCN101085769AReduce pollutionSimple reaction conditionsOrganic chemistryCyclohexanoneState of art
The invention discloses a method for synthesizing alpha- pyranone derivant demonstrated in formula (I). It comprises following steps: carrying out cyclic reaction with affixture of Baylis-Hillman and 1, 3- cyclohexanone and its derivant demonstrated in formula (III) under catalytic action of alkali and with existence of organic disslovant or without disslovant at subzero 20 to 10 Deg. C, reacting for 1- 12 hours, post-treating after reaction and getting said alpha- pyranone derivant. The invention is characterized by easy got raw material, simple and safe operation, temperate reaction condition, high productivity, simple post-treatment, little environmental pollution, and great performing value and social and economic benefit.
Owner:ZHEJIANG UNIV OF TECH
Sulfur-bearing uridine anticancer drug, intermediate and synthesis method
InactiveCN103467549ASmall side effectsHigh value for development research and clinical applicationSugar derivativesEnergy modified materialsAcetic anhydrideLight wave
The invention relates to a synthesis method which comprises the steps of taking uridine as a principal raw material, treating with iodine and dilute nitric acid, obtaining 5-iodine uridine, treating with acetic anhydride to form 2',3',5'-O-trioxide acetyl-5-iodine uridine, allowing 2',3',5'-O-trioxide acetyl-5-iodine uridine to react with 2-(tributyl stannane) furan or thiophene by the action of triphenyl phosphine palladium chloride to form an intermediate, deprotecting by stirring in an ammonia methanol saturated solution at the room temperature by the action of phosphorus pentasulfide, and obtaining 5-(2-furyl or thienyl)-4-sulfur-bearing uridine. The compound has absorption at 363nm, and higher sensitivity to ultraviolet A, can enter inner cells of a tissue and act on cancer cells selectively, and overcomes the disadvantages that a photosensitive reagent for optic treatment at present is not gathered in nuclei and cannot selectively act on the cancer cells. The compound belongs to a novel base sulfur-bearing nucleoside compound, absorption light waves of the compound are in a long wavelength region, and the compound can selectively act on the inner cancer cells of the tissue, has a potential pharmaceutical value, and enters the inner cells of the tissue easily.
Owner:DALIAN UNIVERSITY
Carbon fiber modified with crystalized crosslinkable polyaryletherketone sizing agent and preparation method of carbon fiber
ActiveCN110820315ASimple structureImprove bondingPhysical treatmentCarbon fibresPolymer scienceCarbon fibers
The invention discloses a carbon fiber modified with a crystalized crosslinkable polyaryletherketone sizing agent and a preparation method of the carbon fiber and belongs to technical field of carbonfiber surface treatment. The preparation method includes subjecting double-fluorine monomer containing aniline side groups and bisphenol monomers to polymerization, or modifying crystalized polyaryletherketone, so as to obtain soluble amorphous polyaryletherketone polymer, and blocking thermotropic crosslinking groups to two terminals of the polymer; meanwhile, subjecting the carbon fiber to surface electrochemical reduction, and grafting the crosslinking groups which are the same as the mentioned to the surface of the carbon fiber; further, drafting the carbon fiber which is subjected to thesurface electrochemical reduction to pass through a sizing agent solution to size the carbon fiber, and performing acidification to recover the crystallinity of the polyaryletherketone sizing agent; finally, finishing the carbon fiber. The carbon fiber can be used for preparing a composite material, the composite material is subjected to high-heat treatment, so that the crosslinking reaction is initiated, the crystallinity of the polyaryletherketone polymer is improved, the sizing agent is allowed to have a crystalline texture and can form a chemical bonding with the surface of the carbon fiber, and further, the interference shear strength is improved, and the composite material has high temperature resistance and corrosion resistance performance.
Owner:JILIN UNIV
Method for preparing inorganic compound melamine hard foaming nano-material
The invention discloses a method for preparing an inorganic compound melamine hard foaming nano-material. The method comprises the following steps: A, causing melamine, paraformaldehyde and water to react to produce polyhydroxy melamine; B, adding an inorganic nano-material and a modifying agent into the polyhydroxy melamine to form a prepolymer resin solution; C, adding an emulsifying agent, a foaming agent, a foam stabilizer and a curing agent into the prepolymer resin solution, uniformly stirring, foaming in a microwave oven, and curing to obtain the inorganic compound melamine hard foaming nano-material. According to the method, an inorganic nano-material having an inorganically treated surface and the modifying agent are added into polyhydroxy melamine, so that the inorganic nano-material is directly dispersed in a resin system and participates in an acidic polycondensation process to form a crossed three-dimensional reticular structure with resin, and therefore, the product has the advantages of melamine and the special properties of nano-particles, and has the advantages of high strength, high modulus, good toughness, high temperature resistance and the like on mechanical performance.
Owner:HENAN JUNHUA DEV
Bisphenol fluorene synthesizing process catalyzed with solid supported heteropolyacid
InactiveCN1986509AEasy to recycleThe synthesis process is reasonable and feasibleCatalyst carriersOrganic chemistryHeteropoly acidCarboxylic acid
The bisphenol fluorine synthesizing process includes mixing phenol, 9-fluorenone, solid supported heteropoly acid and mercapto carboxylic acid, with phenol / 9-fluorenone molar ratio of 6-14 to 1, solid supported heteropoly acid accounting for 5.0-20.0 % of total reactant weight, heteropoly acid / solid carrier weight ratio of 0.3-1 to 1 and mercapto carboxylic acid / 9-fluorenone weight ratio of 0.02-0.50 to 1, to react at 60-130 deg.c via stirring for 6-14 hr; filtering the reacted product while it is still hot, and recovering the catalyst; washing the catalyst, merging the washed liquid with the filtrate, crystallizing, filtering, drying, recrystallizing in organic solvent and vacuum drying to obtain bisphenol fluorine crystal. The present invention has product purity as high as 99.8 %, simple post-treatment, less metal corrosion and environmental pollution and recovery of catalyst, and may be used widely in the phenol and 9-fluorenone condensation reaction.
Owner:HARBIN ENG UNIV
Method for utilizing nitrate ions to degrade and decolorize dye
InactiveCN108147495AWide range of raw materialsFast degradationWater/sewage treatment by irradiationWater treatment compoundsHigh concentrationUltraviolet
A method for utilizing nitrate ions to degrade and decolorize dye is characterized by comprising the following steps that (1), nitrate is added into a solution colored by dye, and the concentration ofthe nitrate ions in the solution is made to be 0.01-15g / L; and (2), the solution where the nitrate ions are added in the step (1) is placed in a sunlight or ultraviolet environment with the irradiance being 18300 microwatt / cm<2> to be continuously irradiated. According to the method, high-concentration dye can be effectively degraded only by the nitrate ions under irradiation of sunlight or ultraviolet. The method has the characteristics of being wide in raw material, high in degradation speed, low in cost, gentle in reaction condition, simple in post-treatment, convenient to operate and thelike.
Owner:BENGBU COLLEGE
Schiff base containing carbazyl and thiadiazolyl and preparation method thereof
InactiveCN106432220AOvercome timeTo overcome the large amount of solventOrganic chemistryLuminescent compositionsCarbazoleRoom temperature
The invention relates to Schiff base containing carbazyl and thiadiazolyl and a preparation method thereof; the preparation method comprises: adding acyl carbazole, 2-amino-5-substituted-1,3,4-thiadiazole and p-toluenesulfonic acid, grinding at room temperature, performing TLC (thin layer chromatography) monitoring on reaction until the materials react completely, and standing to obtain a crude product, wherein a molar ratio of the acyl carbazole, 2-amino-5-substituted-1,3,4-thiadiazole and p-toluenesulfonic acid is 1:A:B, and wherein A is 1-1.2 or 2-2.2, and B is 1-1.2 or 2-2.2; subjecting the crude product to washing and suction filtering to obtain the Schiff base containing carbazyl and thiadiazolyl. The reaction time is short, reaction conditions are mild, reacting may be performed at room temperature, equipment requirements are low, post-processing is simple, no solvents are required, and the yield is high; the Schiff base containing carbazyl and thiadiazolyl prepared herein contains multiple C=N fluorescent groups and carbazole groups with good hole transport capacity, and have certain luminescent properties.
Owner:SHAANXI UNIV OF SCI & TECH
4-amino-5-substituted-1,2,4-triazole-3-thione Schiff base and preparation method thereof
The invention relates to a 4-amino-5-substituted-1,2,4-triazole-3-thione Schiff base and a preparation method thereof. The preparation method comprises: adding A mol of 4-amino-5-substituted-1,2,4-triazole-3-thione, B mol of benzaldehyde or substituted benzaldehyde and C mol of p-toluene sulfonic acid to a dried reaction container, grinding the raw materials at a room temperature until the raw materials completely react, and standing to obtain a crude product, wherein a ratio of A to B to C is 1:(1-1.2):(1-1.2); and dissolving the crude product with a solvent, carrying out suction filtration, and concentrating the filtrate until achieving a dry state to obtain the 4-amino-5-substituted-1,2,4-triazole-3-thione Schiff base. According to the present invention, the preparation method adopts the solid phase reaction, the reaction time is short, the reaction conditions are mild, the equipment requirements are low, the operations are simple, the post-treatment is simple, the solvent is not required, characteristics of green, economy and environmental protection are provided, and the yield of the target product is up to more than 86%.
Owner:SHAANXI UNIV OF SCI & TECH
Schiff base containing carbazolyl group and oxadiazole group and preparing method thereof
InactiveCN106432217AHigh yieldShort reaction timeOrganic chemistryLuminescent compositionsFluorescenceChemistry
The invention relates to a schiff base containing a carbazolyl group and an oxadiazole group and a preparing method thereof. The method includes the steps that acylcarbazole, 2-amino-5-substituted-1,3,4-oxadiazole and p-toluenesulfonic acid are added into a dry reaction container and ground under the room temperature condition, TLC is used for monitoring the reaction until the raw materials react completely, and a crude product is obtained after standing, wherein the molar ratio of acylcarbazole: 2-amino-5-substituted-1,3,4-oxadiazole: p-toluenesulfonic acid is 1:A:B, wherein the range of A is 1-1.2 or 2-2.2, and the range of B is 1-1.2 or 2-2.2; the schiff base containing the carbazolyl group and the oxadiazole group is obtained after the crude product is washed and filtered in a suction mode. The preparing method is high in reactivity, high in reaction speed and short in reaction time, and the schiff base containing the carbazolyl group and the oxadiazole group contains multiple C=N fluorescent groups and the carbazole group with high hole-transport capacity and has a certain luminescence property.
Owner:SHAANXI UNIV OF SCI & TECH
Method for preparing carbonyl ferrocene condensed 2-amino-5-substituted-1,3,4-thiadiazole
The invention discloses a method for preparing carbonyl ferrocene condensed 2-amino-5-substituted-1,3,4-thiadiazole. The method comprises the following steps: adding A mol of carbonyl ferrocene, B mol of 2-amino-5-substituted-1,3,4-thiadiazole and C mol of p-toluenesulfonic acid into a dried mortar, grinding at room temperature until the raw material reaction (a TLC monitoring reaction) is complete, preserving the temperature in a drying box under the condition of 50 DEG C for 30 minutes, cooling to room temperature, adding absolute ethyl alcohol, performing suction filtration on the mixed solution, removing the catalyst p-toluenesulfonic acid, performing vacuum concentration until the filtrate is dried, thereby obtaining the crude product, wherein the ratio of A to B to C is 1:(1.0-1.2):(1.0-1.2); and recrystallizing the crude product by using absolute ethyl alcohol, thereby obtaining the purified product. The method disclosed by the invention is short in reaction time, mild in reaction conditions, low in equipment requirements, easy to operate and simple in after-treatment and is a green, economic, environment-friendly and high-efficiency method for synthesizing the carbonyl ferrocene condensed 2-amino-5-substituted-1,3,4-thiadiazole, a solvent is not needed, the catalyst can be repeatedly used, and the yield is over 85 percent.
Owner:SHAANXI UNIV OF SCI & TECH
Preparation method of cyanomethyl ester
InactiveCN105294495AIncrease profitNo generationCarboxylic acid nitrile preparationOrganic compound preparationSodium acetatePtru catalyst
The invention discloses a preparation method of cyanomethyl ester. In the presence of an oxidizing agent, a carboxylic acid compound and cyanoacetic acid are used as reactants, iodide is used as a catalyst, and sodium acetate is used as alkali, so as to prepare the cyanomethyl ester in a mixed solvent through nucleophilic substitution. According to the method, the reactivity of the catalyst is high, reaction conditions are mild, the application range of substrates is wide, the postprocessing is convenient, the yield of target products is high, a preparation process is simple, green and environmentally friendly, and the sources of used raw material are wide.
Owner:SUZHOU UNIV
nnn ligand, its metal complex, preparation method and application
ActiveCN105294667BMild preparation methodEasy to prepareIron organic compoundsCobalt organic compoundsRegioselectivityCombinatorial chemistry
The invention discloses an NNN ligand, metal complexes thereof, preparation methods and application, and particularly provides an NNN ligand 1, a metal complex 2 of the NNN ligand, a metal complex 3 of the NNN ligand and preparation methods of the NNN ligand 1 and the metal complexes, as well as application of the metal complex 3 of the NNN ligand to catalysis on hydroboration reaction of bis-substituted olefin, especially application of the metal complex 3 to catalysis on asymmetric hydroboration reaction of 1, 1-bis-substituted olefin. The metal complex 3 of the NNN ligand has good catalytic activity in the hydroboration reaction of the bis-substituted olefin, especially asymmetric hydroboration reaction of the 1, 1-bis-substituted olefin, has excellent regioselectivity and enantioselectivity, and is high in yield and mild in reaction conditions; besides, the preparation methods of the NNN ligand and the metal complexes thereof are simple, environment-friendly, mild in reaction conditions, relatively high in yield, and simple in post-processing, and the raw materials are low in cost and easy to obtain, so that the preparation methods are suitable for industrial production. (The formulas of the NNN ligand 1, metal complex 2 and metal complex 3 are shown in the description).
Owner:SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
Method for synthesizing compound ticagrelor and synthesized intermediate thereby
ActiveCN107513070AMild reaction conditionsSimple reaction conditionsOrganic chemistryTicagrelorCombinatorial chemistry
The invention discloses a method for synthesizing a compound ticagrelor and a synthesized intermediate thereby. The method comprises the following steps: carrying out a substitution reaction between a compound (2) and a compound (3) to prepare a compound (4); carrying out a reduction reaction on the compound (4) to prepare a compound (5); carrying out a chlorination reaction on the compound (5) to prepare a compound (6); carrying out a substitution reaction between the compound (6) and a compound (7) to prepare a compound (8); and finally, carrying out a hydroxyl deprotection reaction on the compound (8), thereby obtaining the ticagrelor (1). The reaction formulas are as shown in the specification. The invention provides a novel method for synthesizing ticagrelor. The synthetic method has the advantages of novel technical route, simple and convenient operation, high synthesis yield, high product purity, cheap and readily available raw materials and the like, and is suitable for industrialized production. Meanwhile, the synthesized ticagrelor intermediate provides a novel intermediate raw material for preparation of the ticagrelor.
Owner:HUAIYIN INSTITUTE OF TECHNOLOGY
Supported catalyst and application thereof in preparation of hydroxyalkyl acrylate
ActiveCN111185205AEasy to operateMild conditionsPhysical/chemical process catalystsOrganic compound preparationPtru catalystHigh activity
The invention discloses a supported catalyst and application thereof in preparation of hydroxyalkyl acrylate. The catalyst is obtained by loading any elemental substance of magnesium, calcium, iron, copper, zinc or aluminum, oxide, sulfate and halide onto a carrier, wherein the weight ratio of the elemental substance of magnesium, calcium, iron, copper, zinc and aluminum, the oxide, the sulfate and the halide is 1:(1-3):(1-10):(1-5), and the weight of the carrier is 1-5 times of the total weight of the elemental substance of magnesium, calcium, iron, copper, zinc and aluminum, the oxide, the sulfate and the halide. The catalyst used in the invention has the advantages of cheap and easily available components, low manufacturing cost, simple operation process, mild conditions, convenient post-treatment, high activity, long service lifetime, and capable of being regenerated and reused. The process of utilizing the catalyst for preparing hydroxyalkyl acrylate is simple, the production process is safe, no polymerization inhibitor is needed, continuous operation can be performed, the raw material conversion rate is 96% or above, and the product purity is 99% or above.
Owner:CHIZHOU FANGDA SCI & TECH CO LTD
Phosphine pyridine oxazoline compound, metal complex, and preparation method and application thereof
ActiveCN111690009AHigh yieldMild reaction conditionsSilicon organic compoundsGroup 5/15 element organic compoundsAsymmetric hydrogenationCombinatorial chemistry
The invention discloses a phosphine pyridine oxazoline compound, a metal complex, and a preparation method and application thereof. According to the invention, the preparation methods of the phosphinepyridine oxazoline compound and the metal complex are simple, wherein the raw materials are cheap and easy to obtain, the process is environmentally friendly, reaction conditions are mild, the yieldis high, aftertreatment is simple, and large-scale production is easy. The phosphine pyridine oxazoline compound has chiral induction capability and can be complexed with metal cobalt or iron to forma chiral metal complex of the phosphine pyridine oxazoline compound. The metal complex disclosed by the invention has excellent catalytic activity in asymmetric hydrogenation reaction of alpha-alkenylsilicon, particularly in asymmetric hydrogenation reaction of alpha-silicon-based styrene compounds, and is excellent in enantioselectivity, high in yield and mild in reaction condition.
Owner:SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
Alkyl-substituted ethyl acetate-based guanidine ionic liquid as well as preparation and application thereof
ActiveCN111393332AHigh catalytic activityThe synthesis process is simpleOrganic compound preparationOrganic-compounds/hydrides/coordination-complexes catalystsMethylanilineDimethylaniline N-oxide
The invention discloses alkyl-substituted ethyl acetate-based guanidine ionic liquid as well as preparation and application thereof, which are characterized in that tetramethylguanidine and 2-bromo ester are ionized to obtain alkyl-substituted ethyl acetate-based guanidine ionic liquid, and the alkyl-substituted ethyl acetate-based guanidine ionic liquid is applied as a catalyst to formylation and methylation reactions of carbon dioxide, N-methylaniline and derivatives of the N-methylaniline to selectively generate N-methylformylaniline or N, N-dimethylaniline and derivatives thereof. Compared with the prior art, the alkyl-substituted ethyl acetate-based guanidine ionic liquid has the advantages of good catalytic performance, mild reaction conditions, simple post-treatment, simple synthesis, low cost, greenness and high efficiency, avoids the use of a large amount of organic solvents when being used as a solvent and a catalyst at the same time, and has important meanings in the research of medicinal chemistry and medical intermediate compounds.
Owner:EAST CHINA NORMAL UNIV
Preparation method of high molecular weight branched polymers
Belonging to the field of polymer synthesis, the invention relates to a preparation method of high molecular weight branched polymers. The method includes: taking an alcoholic hydroxyl monomer as a hydroxyl monomer, adopting acrylic ester as a double-bond monomer, catalyzing the Oxa-Michael addition polymerization of hydroxyl and unsaturated double or triple bond in an organic solvent by organophosphorus nitrile base t-BuP2, thus preparing high molecular weight branched polymers with different terminal groups. The branched polymers prepared by the method provided by the invention have the characteristics of controllable and modifiable structure, and are suitable for application in different fields. The method has the advantages of mild reaction conditions, fast reaction, high efficiency and high yield, and the required monomers are all commercial monomers, the catalyst is free of metal residue, safe and environment-friendly, therefore the high molecular weight branched polymers can beused for large-scale production and application, and have huge application prospects.
Owner:CHANGZHOU UNIV
Synthesis method of 1,4-butylene glycol dimethacrylate
InactiveCN110668939AReduce energy consumptionEasy to separateOrganic compound preparationCarboxylic acid esters preparationMethacrylatePtru catalyst
The invention discloses a synthesis method of 1,4-butylene glycol dimethacrylate, and belongs to the field of organic chemical industry. The synthesis method includes the steps that when reaction rawmaterials: 1,4-butanediol, methacrylic acid, a polymerization inhibitor and a water-carrying agent are heated to 80-90 DEG C, an HZSM-5 molecule sieve is added to serve as a catalyst, the temperatureis increased and kept to be 100-130 DEG C, the 1,4-butanediol and the methacrylic acid are subjected to an esterification reaction to generate 1,4-butylene glycol dimethyl alkenyl benzoate; after thereaction is completed, cooling is conducted to the room temperature, the catalyst is filtered and separated, still standing for layering is conducted in a separating funnel, and an upper layer organicphase is taken; the organic phase is washed with distilled water for 2-3 times; and then vacuum distillation is conducted to remove an organic solvent, and after cooling, a target product, namely the1,4-butylene glycol dimethacrylate is obtained. The catalyst has high activity, good selectivity, the mild reaction condition, easy and convenient post-treatment and no corrosivity, and is easy to separate and capable of being reused, and thus the synthesis method is high in production safety, low in energy consumption and high in yield.
Owner:JIANGSU ZHENGDAN CHEM IND CO LTD
NCP ligand, metal iridium complex thereof, and preparation method and application of complex
ActiveCN113861243AChiral inducing abilityHigh catalytic activityIndium organic compoundsOrganic compound preparationArylHydrogenation reaction
The invention discloses an NCP ligand, a metal iridium complex thereof, and a preparation method and application of the complex. The NCP ligand has a structure as shown in a formula 1, and can be complexed with metal iridium to form the chiral metal iridium complex of the NCP ligand as shown in a formula 2, and the complex has excellent catalytic activity in hydrogenation reaction of diaryl substituted olefin, and has the advantages of better regioselectivity, better enantioselectivity, high yield, mild reaction conditions and the like especially in asymmetric transfer hydrogenation reaction.
Owner:SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
Preparing method for 1-(N-alkylphenothizainyl)-1-methyl(H)-2-substituted Schiff base
The invention relates to a preparing method for a 1-(N-alkylphenothizainyl)-1-methyl(H)-2-substituted Schiff base. The preparing method includes the steps that A mol of 3-formyl(acetyl)-N-alkyl phenothiazine, B mol of substituted ammonia and C mol of p-toluenesulfonic acid are added into a dry reaction container and ground on the room temperature condition, TLC is used for monitoring reactions until the raw materials react completely, and a crude product is obtained after standing, wherein the ratio of A:B:C is 1:(1-1.2): (1-1.2); water scrubbing and suction filtration are carried out on the crude product to obtain the 1-(N-alkylphenothizainyl)-1-methyl(H)-2-substituted Schiff base. The solid-phase reactions are involved in the preparing method and short in reaction time and moderate in reaction condition, the preparing method is low in requirement for equipment, easy to operate, simple in aftertreatment, environmentally friendly, economical and efficient and does not need solvent, and the yield of the target product reaches up to 80% or more.
Owner:SHAANXI UNIV OF SCI & TECH
A kind of preparation method of 7,8-dihydroquinoline-2,5(1h,6h)-dione derivatives
InactiveCN101260079BReduce pollutionRaw materials are easy to getOrganic chemistryPtru catalystOrganic solvent
The invention discloses a preparation method of a 7,8-dihydroquinoline-2,5(1H,6H)-dione derivative represented by formula (I), the preparation method comprising the following steps: as shown in formula (I) The Baylis-Hillman adduct represented by (II) reacts with 1,3-cyclohexanedione represented by formula (III) or 1,3-cyclohexanedione represented by formula (III) under the action of a base catalyst at 0~100°C in an organic solvent or under solvent-free conditions. The derivative is reacted for 1-12 hours, then primary amine is added to react at 0-100° C. for 1-8 hours, and the compound of formula (I) can be obtained after post-treatment. Compared with the prior art, the present invention is mainly embodied in easy availability of raw materials, simple and convenient operation, mild reaction conditions, high reaction yield, good atom economy, and low environmental pollution, so it has greater practical value and potential social and economic benefits.
Owner:ZHEJIANG UNIV OF TECH
A kind of preparation method of dihydropyridine crude drug
The invention relates to a preparation method of a dihydropyridine raw material drug, comprising the following steps: putting ethyl acetoacetate and urotropine into a reaction kettle, mixing them at 15-20°C; slowly adding ethanolamine dropwise, and raising the temperature after the dropwise addition Reaction: cool down to crystallize, centrifuge to obtain crude dihydropyridine; add ethanol and crude dihydropyridine to the refining kettle, heat and stir to dissolve, adjust pH to neutral with glacial acetic acid, add activated carbon, stir for 1 hour, and then press into Crystallization kettle; crystallization at lower temperature, centrifugation, and vacuum drying to obtain dihydropyridine raw material medicine. The reaction process of the invention does not use organic solvents, has simple operation, less environmental pollution, mild reaction conditions, high safety, low cost, good product quality and is beneficial to industrialization.
Owner:河南豫辰药业股份有限公司
A kind of synthetic method of compound ticagrelor and its synthetic intermediate
ActiveCN107513070BMild reaction conditionsSimple reaction conditionsOrganic chemistryTicagrelorSynthesis methods
The invention discloses a method for synthesizing a compound ticagrelor and a synthesized intermediate thereby. The method comprises the following steps: carrying out a substitution reaction between a compound (2) and a compound (3) to prepare a compound (4); carrying out a reduction reaction on the compound (4) to prepare a compound (5); carrying out a chlorination reaction on the compound (5) to prepare a compound (6); carrying out a substitution reaction between the compound (6) and a compound (7) to prepare a compound (8); and finally, carrying out a hydroxyl deprotection reaction on the compound (8), thereby obtaining the ticagrelor (1). The reaction formulas are as shown in the specification. The invention provides a novel method for synthesizing ticagrelor. The synthetic method has the advantages of novel technical route, simple and convenient operation, high synthesis yield, high product purity, cheap and readily available raw materials and the like, and is suitable for industrialized production. Meanwhile, the synthesized ticagrelor intermediate provides a novel intermediate raw material for preparation of the ticagrelor.
Owner:HUAIYIN INSTITUTE OF TECHNOLOGY
Method for synthesizing alpha-pyranone derivatives
InactiveCN101085769BReduce pollutionSimple reaction conditionsOrganic chemistryCyclohexanoneState of art
The invention discloses a method for synthesizing alpha- pyranone derivant demonstrated in formula (I). It comprises following steps: carrying out cyclic reaction with affixture of Baylis-Hillman and1, 3- cyclohexanone and its derivant demonstrated in formula (III) under catalytic action of alkali and with existence of organic disslovant or without disslovant at subzero 20 to 10 Deg. C, reactingfor 1- 12 hours, post-treating after reaction and getting said alpha- pyranone derivant. The invention is characterized by easy got raw material, simple and safe operation, temperate reaction condition, high productivity, simple post-treatment, little environmental pollution, and great performing value and social and economic benefit.
Owner:ZHEJIANG UNIV OF TECH
Preparation method of adipic acid
ActiveCN113548958AReduce pollutionMild reaction conditionsOrganic compound preparationCarboxylic preparation by oxidationCyclohexanonePhotosensitizer
The invention discloses a preparation method of adipic acid. Cyclohexanone is used for synthesizing adipic acid under the irradiation of visible light, the catalysis of a photosensitizer and the oxidation environment of air, oxygen or hydrogen peroxide, the reaction conditions are mild, the reaction efficiency is high, and the cost is low. In addition, the reaction can pass through a continuous flow reactor, the reactant dosage is increased, the reaction efficiency is improved, the reaction time is shortened, and a foundation is laid for further industrial production.
Owner:XI AN JIAOTONG UNIV
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