88 results about "DABCO" patented technology

The invention relates to a synthetic process of a chemical substance, and particularly relates to a synthetic method for synthesizing (E)-2-[2-(6-chloro pyrimidine-4-yloxy)phenyl]-3-methoxy methacrylate and azoxystrobin; the method comprises the following steps: mixing a raw material of 3-(alpha-methoxy)methylene benzofuran-2-(3H)-ketone and potassium carbonate in a toluene solvent, cooling to 0-10 DEG C, adding sodium methoxide, reacting for 0.4-0.6 hours; adding 4,6-dichloropyrimidine and a catalyst of DABCO, reacting for 1-2 hours, filtering to remove inorganic salts, washing the filtrate with water, performing distillation to recover toluene; adding a catalyst of potassium bisulfate into the distillation residues of the above reaction, heating to 132-145 DEG C in a reduced-pressure condition for reaction; directly adding salicylonitrile to synthesize azoxystrobin or performing toluene dissolution, water washing, solvent recovery, recrystallization and filtration to obtain an intermediate. The production and synthesis of (E)-2-[2-(6-chloro pyrimidine-4-yloxy)phenyl]-3-methoxy methacrylate by the production process of the invention has high yield, and simple operations, and the used raw materials and processes are routine reagents and methods.

The invention relates to a preparation method of a MOFs (Metal-Organic Frameworks) graphene composite material, comprising the following steps: (1) preparing graphene by taking graphite oxide as a raw material, THF (tetrahydrofuran) as a reaction medium and NaBH4 as a reducing agent; (2) adding graphene, metal salt, H2BDC (1,4-benzenedicarboxylic acid) and DABCO (1,4-diazabicyclooctane triethylenediamine) into a THF/H2O/CH3OH mixed solution, ultrasonically stirring, reacting for 12-72 h at 80-180 DEG C, and purifying to obtain the MOFs-graphene composite material. According to the preparation method, in the step (1), the experimental condition for preparing a graphene precursor is mild, the time is short, the number of layers of the prepared graphene is small, the use level of the reducing agent is reduced as THF is used as a solvent, high temperature is not needed, complex washing and drying processes are eliminated, and the environment pollution is less; in the step (2), the THF is used as an organic solvent for synthesis of the metal organic frameworks, the utilization rate of the raw material is increased, the THF solvent is low in boiling point and low in usage requirement on equipment, and an after-treatment process is simple and easy to operate. The MOFs-graphene composite material prepared by the method can be widely applied to energy devices such as a fuel-cell catalyst, a super-capacitor, and an anode material and an adsorbing material of a lithium ion battery.

An oxygen sensitive ink or coating with enhanced photostability, comprising an oxygen sensitive indicator, a photostabilizer, an oxygen permeable binder and a solvent mixture is provided. The oxygen sensitive indicator is selected from, but not limited to [Ru(L1)(L2)(L3)]²⁺, wherein Ru represents the central ruthenium ion, L1, L2 and L3 represent the bidentate ligands diphenylphenanthroline, phenanthroline or bipyridine ligands or optionally substituted variations of same with representative counter ions selected from (PF6)-, Cl—, BF4-, Br— and (Cl04)-, platinum or palladium based metallo-porphyrin. The photostabilizer is selected from, but not limited to CIBA TINUVIN 5236, TINUVIN 292, TINUVIN 123 and TINUVIN 272, TINUVIN 477W, DABCO and ascorbic acid. Oxygen sensitive elements incorporating the oxygen sensitive ink or coating are manufactured by printing on a continuous flexible or rigid substrate using printing method including ink-jet, gravure, flexographic, pad printing or pin printing.

The invention provides a long side chain SEBS-based alkaline polymer electrolyte membrane, a preparation method and applications thereof, wherein the long side chain SEBS-based alkaline polymer electrolyte membrane is prepared by grafting a long side chain polymer material, the grafted long side chain has a positively charged functional group, the positively charged functional group is one or twoselected from quaternary ammonium salt ions, imidazole salt ions, guanidine salt ions and DABCO(1,4-diazabicyclo[2.2.2]octane) ions, and the long side chain is C2-C8 long alkyl chain. According to thepresent invention, SEBS with good mechanical property and good chemical stability is used as the main chain of the long alkyl chain alkaline polymer electrolyte membrane, such that the membrane has good mechanical property, has good chemical stability in the high temperature alkaline environment, and can meet the requirements of the fuel cell working environment; and the large-area membrane can be prepared by simply adjusting the temperature and the pressure through the hot pressing or solvent method, such that the membrane casting process is simple, and the batch production is easily achieved.

An oxygen sensitive polymeric material with enhanced photostability, comprising an oxygen sensitive indicator and photostabilizer incorporated into an oxygen permeable polymeric material is provided. The oxygen sensitive indicator can be, but is not limited to, [Ru(L1)(L2)(L3)]²⁺, wherein Ru represents the central ruthenium ion, L1, L2 and L3 represent the bidentate ligands diphenylphenanthroline, phenanthroline or bipyridine ligands or optionally substituted variations of same with representative counter ions selected from (PF6)—, Cl—, BF4—, Br— and (C 104)—, platinum or palladium based metallo-porphyrin. The photostabilizer is selected from CIBA TINUVIN 5236, TINUVIN 292, TINUVIN 123 and TINUVIN 272, TINUVIN 477W, DABCO and ascorbic acid. A sensor system for detecting oxygen and a method for detecting oxygen in a package is also provided.

The invention belongs to the technical field of organic compounds and particularly provides beta-trifluoromethyl vinyl sulfone compounds, a preparation method thereof and an application of the compounds to tumor cell proliferation resistance. The beta-trifluoromethyl vinyl sulfone compounds are prepared from a multicomponent reagent (trifluoromethyl) trimethylsilane (TMSCF3), alkyne, diazonium salt and DABCO.(SO2)2 in an organic solvent DMSO through a one-step reaction. Reaction conditions are quite mild, alkyne bi-functionalization is realized directly through the one-step cascade reaction of the four raw materials, the operation is simple, defects of tedious steps, low operability and yield and poor selectivity of the traditional synthesis method of vinyl sulfone derivatives are overcome, and the method is applicable to large-scale preparation and has quite good application prospect. In-vitro pharmacological activity screening tests show that the compounds have an anti-proliferation effect on tumor cells, part of the compounds have an obvious tumor inhibition activity, the half maximal inhibitory concentration IC50 value can reach mu m level, and the compounds can be used for preparing a kind of novel anti-tumor reagents.

STA-19, a molecular sieve having a GME structure and phosphorus in the framework, is described. STA-19AP (as prepared) can have a lower alkyl amine, such as trimethylamine, and olig-(1,4-diazabicyclo[2.2.2]octane)-pentyl dibromide ([DABCO-C5]_x where x represents the number of repeating units) or olig-(1,4-diazabicyclo[2.2.2] octane)-hexyl dibromide ([DABCO-C6]_x) as SDAs. A lower alkyl ammonium hydroxide, such as tetrabutylammonium hydroxide (TBAOH), can be used as a pH modifier for the preparation of SAPO-STA-19. A calcined product, STA-19C, formed from STA-19AP is also described. Methods of preparing STA-19AP, STA-19C and metal containing calcined counterparts of STA-19C are described along with methods of using STA-19C and metal containing calcined counterparts of STA-19C in a variety of processes, such as treating exhaust gases and converting methanol to olefins are described.

The invention provides a long side chain SEBS base alkaline polymer electrolyte membrane as well as a preparation method and application thereof. The SEBS base alkaline polymer electrolyte membrane has a long side chain structure, a positively-charged functional group in the structure is one of or more than two of quaternary ammonium salt, imidazolium salt, guanidine salt and DABCO (1,4-diazabicyclo (2.2.2) octane); the long side chain is an oxygen-containing long alkyl chain of C2-C8. The oxygen-containing long alkyl chain SEBS-base alkaline polymer electrolyte membrane prepared by the preparation method provided by the invention has better chemical stability in a high-temperature alkaline environment due to the selection of an SEBS main chain with good chemical stability and the design of a polymer molecular structure with the functional group away from the long side chain; the oxygen-containing long alkyl chain is prepared through reactant selection, reaction temperature control andoptimization of ratio among reactants; by further adopting a hot pressing or solvent evaporation method, the oxygen-containing long alkyl chain SEBS base alkaline polymer electrolyte membrane with auniform, smooth and compact surface can be prepared through controlling the casting temperature, a solvent or the pressure.

The invention discloses a method for synthesizing a key intermediate of an antitumour medicament Romidepsi, comprising the following steps of: with PyBop as a condenser, carrying out condensation on L-Val-OMe and Fmoc-L-Thr by dehydrating, removing a Fmoc protective group with diethylamine, carrying out condensation on the obtained dipeptide and N-Boc-D-Cys(Trt), reacting the obtained tripeptide with para-toluenesulfonic acid anhydride, then adding DABCO (1,4-Diazabicyclo[2.2.2]octane), and carrying out elimination reaction by virtue of E1 to form tripeptide containing double bonds; removing a Boc protective group with boron trifluoride etherate, and condensing Fmoc-D-Val with tripeptide the terminal of which is a free amino group to obtain the key intermediate of Romidepsi, wherein the structure of the key intermediate is shown by a formula (described in the specification). According to the method disclosed by the invention, two commercial L-type amino acids and two commercial D-typeamino acids are taken as raw materials, a classical peptide condensing agent is utilized, and the key intermediate is obtained at high total yield of 63.8% and can be directly applied to the next synthesis step of Romidepsi.

The invention relates to the field of electrochemistry, in particular to an electrolyte solute for a high-voltage supercapacitor, an electrolyte and the high-voltage supercapacitor applying the electrolyte. Anion of the electrolyte solute can be selected from one or more of tetrafluoroborate, hexafluorophosphate, bis(trifluoroMethylsulfonyl)imino, bis(trifluoroMethylsulfonyl)methyl and perfluoro alkyl sulfonic acid, and cation can be selected from one or more of N-methyl-1,4-diazabicyclo[2.2.2] ammonium octane, N,N-dimethyl-1,4-diazabicycle[2.2.2] ammonium octane and N-methyl-1-diazabicyclo[2.2.2] ammonium octane. The high-voltage supercapacitor made of the electrolyte which is prepared from the electrolyte solute can stably work for a long time at voltages of 2.7 to 3.2V, energy density is greatly improved, the characteristic of high power density of the high-voltage supercapacitor is kept, and the service life of the high-voltage supercapacitor is prolonged.

The invention relates to a simple and novel method for synthesizing spiro[oxoindole-3,5'-oxazoline] heterocyclic compound. The spiro[oxoindole-3,5'-oxazoline] heterocyclic compound in the invention has a structural formula as represented by Fig. I. According to the invention, isatin or substituted isatin is used as a raw material, DABCO is used as alkali, and tetrahydrofuran and water (in a ratio of 1:2) are used as a mixed solvent, and the spiro[oxoindole-3,5'-oxazoline] heterocyclic compound substituted by a plurality of functional groups can be obtained in one step through Aldol condensation reaction and a cyclization reaction among the above-mentioned raw materials and isonitrile (wherein, the weight ratio of isatin to isonitrile is 1.2:1). According to the method, the reactions are simple, high yield is obtained, and a water/organics solvent is used to substitute commonly used organic solvents, being in accordance with requirements of green chemistry. Furthermore, a product of chiral spiro[oxoindole-3,5'-oxazoline] with a high d.r value and ee value can be obtained by using a chiral catalyst. The method provided in the invention enables rapid and large-scale synthesis of a library of various substituted spiro[oxoindole-3,5'-oxazoline] heterocyclic compounds to be realized and allows discovery of drug lead compounds to be accelerated.

The invention relates to a preparation method of a 5-aryl-3-trifluoromethyl-1H-pyrazole compound. The preparation method comprises the steps of: adding a catalyst, alkali and DABCO(1,4-diazabicyclo[2,2,2]octane) into a drying reactor, continuously adding 2-aryl-1-acetylene and 2,2,2-trifluoromethyl diazoethane into an organic solvent for completely reacting for 3-24h at the temperature of 0-50 DEG C, and washing, extracting and separating to obtain the 5-aryl-3-trifluoromethyl-1H-pyrazole compound, wherein the molar ratio of the 2-aryl-1-acetylene to the catalyst to the alkali to the DABCO to the 2,2,2-trifluoromethyl diazoethane is 1:(1-3):(1-3):(0.1-1):(2-10). The preparation method provided by the invention is simple, convenient and efficient for synthesizing trifluoromethyl pyrazole compounds and has the advantages of simplicity of operation, mild reaction condition, high yield, good substrate universality and high atom utilization rate.

The invention relates to a preparation method for metal-free perovskite quantum dots DABCO-NH4X3 (X=Cl, Br, I). The preparation method comprises the following steps: (1) dissolving NH4X (X=Cl, Br, I)solids in a mixed solution of N-N dimethylformamide and HX acid, then adding a certain amount of oleic acid and n-octylamine in the mixed solution; (2) adding DABCO (diazabicyclooctane) solids to theprecursor solution, fully reacting, adding ethyl acetate and rapidly producing white solids; and (3) washing and performing centrifugation with cyclohexane, and carrying out vacuum drying to obtain afinished product. According to the invention, long-chain oleic acid and n-octylamine are utilized to control the reaction process of NH4X and DABCO at room temperature effectively, finally the metal-free perovskite quantum dots DABCO-NH4X3 are prepared. The method has the advantages of short reaction time, simple operation, low cost and the like, and is a novel preparation method for the DABCO-NH4X3 quantum dots.

The invention discloses a synthesis method of a beta-hydroxyl substituted sulfonyl compound. The synthesis method of the beta-hydroxyl substituted sulfonyl compound comprises the following steps: catalyzing reaction of phenylhydrazine and DABCO.(SO2)2 in the air by copper salt in an organic solvent and at room temperature to generate sulfonylfree radical so as to perform free radical addition on olefin; and then combining with oxygen molecules in the air to form a peroxide intermediate and performing catalytic reduction to prepare the beta-hydroxyl substituted sulfonyl compound. According to the method, the beta-hydroxyl substituted sulfonyl compound is constructed at one step by utilizing an olefin bifunctionalization strategy under very mild condition, and the functional group diversityof the sulfonyl compound is enriched; the reaction raw materials are simple and easily available; and the method is low in cost, simple to operate and suitable for large-scale preparation, and has good application prospect.

The invention discloses a method for synthesizing a 2-hydroxymethyl acrylate compound, which is characterized by dropwise adding the aqueous solution of formaldehyde into THF solution of acrylate and a catalyst triethylenediamine (DABCO), stirring the mixture to react, adjusting the pH value of the system in the process of reaction, after reaction, obtaining the product through post-treatment. The method effectively improves the defect that the traditional Baylis-Hillman reaction is slow and low in product yield, and has the characteristics of simple operation, low production cost, short production cycle, good product quality, etc.

The invention relates to a novel synthesis method for dialkyl diboronic acid esterification fluorene. The combination of palladium catalysts such as PdCl2 (dppf) and amine substances containing nitrogen ligands such as triethylenediamine (DABCO) or formamine (methenamine) and so on is taken as a catalytic system of the reaction, and methylbenzene is taken as a solvent to be continuously heated and stirred to react for certain hours under the protection of nitrogen atmosphere to successfully realize the boric acid esterification of dibromodialkylfluorene and realize the transformation of a synthesis process of the boric acid esterification of the dibromodialkylfluorene. Compared with the prior butyl lithium method, the method has the advantages that: (1) reaction conditions are easier to obtain, and the reaction operation is simple; (2) the experimental operation has high safety; (3) the reaction time is greatly reduced; and (4) the obtained product has high yield. The method also has the advantages that the method has an advanced process route, reasonable industrial conditions, simple and safe experimental operation, higher product yield, and larger practical value, and is a more ideal synthesis route.

The invention discloses a method for preparing a tetracyclic spiroindoline compound. The method comprises the following steps: adding [SO2], indole alkyne amide, an additive and a photocatalyst into an organic solvent, and conducting reacting under illumination to obtain the tetracyclic spiroindoline compound (with a structural formula as shown in the specification), wherein a molar ratio of [SO2] to indole alkyne amide is 10: 1 to 1: 10; a molar ratio of the [SO2] to the additive is 100: 1 to 1: 10; a molar ratio of the [SO2] to the photocatalyst is 500: 1 to 10: 1; and [SO2] is DABCO.SO2, sodium pyrosulfite, sodium hydrosulfite or sodium hydrogen sulfite. According to the preparation method, cheap inorganic salt is used as a sulfonylation reagent, transition metal catalysis is not needed, strict anhydrous conditions and low-temperature and high-temperature operation are not needed, dangerous peroxides are not needed, expensive photocatalysts are not needed, operation is simple, and cost is low.

The invention belongs to the technical field of preparing methods of polyfunctional group compounds and particularly relates to a method for using deep eutectic solvent for preparing 2-(4-chlorphenyl-hydroxyl methyl)-acrylonitrile. The method mainly solves the problems that when an existing method for preparing 2-(4-chlorphenyl-hydroxyl methyl)-acrylonitrile is used, environment is polluted, and economic benefits are poor. According to the method, choline chloride and glycerin are mixed according to a certain ratio at the temperature of 95 DEG C to prepare the deep eutectic solvent, and then the deep eutectic solvent and water are combined according to the ratio to prepare complex solvent. As the raw materials used for preparing the complex solvent are compounds free of toxicity or low in toxicity, the compound solvent is an environment-friendly medium. The compound solvent is used as a reaction medium and applied to a Morita-Baylis-Hillman (M-B-H) reaction of p-chlorobenzaldehyde and acrylonitrile, wherein DABCO is used for catalyzing the M-B-H reaction, the reaction yield is up to 95%, reaction time is shortened greatly to be a few minutes, most importantly, treatment after the reaction is easy, and a pure target product can be obtained just by simple filtering and washing.

The invention discloses a preparation method MOF@MOF nanometer fiber composite catalyst, and applications of the MOF@MOF nanometer fiber composite catalyst in catalysis of room temperature nitrogen gas into ammonia through reduction, and belongs to the technical field of electrocatalysis and nanometer composite material. The preparation method comprises following main steps: a 1,3,5-benzenetricarboxylic acid ligand solution, a cobalt nitrate solution, and a sodium carbonate solution are mixed to be uniform at room temperature so as to obtain a Co<3>(BTC)<2>*12H<2>O nanometer fiber material; the Co<3>(BTC)<2> nanometer fiber material and a copper acetate-terephthalic acid-triethylenediamine mixed solution are mixed so as to obtain a Co<3>(BTC)<2>*12H<2>O nanometer fiber epitaxial growth [Cu<2>(BDC)<2>(dabco)]DMF*3H<2>O composite material; and the composite material is placed in a microwave oven for 3min of activation at 250W so as to obtain the MOF@MOF nanometer fiber composite catalyst. The MOF@MOF nanometer fiber composite catalyst is used in catalysis of room temperature nitrogen gas into ammonia through reduction, the catalyst preparation cost is low, technology is simple, consumed time is short, and the industrial prospect is promising.

The invention discloses a polyacid supramolecular crystal material and a preparation method thereof. The preparation method comprises the following steps of (1) dropwise adding 50mL of a solution A and 50mL of a solution B into a beaker at a speed of 29-31 seconds/drop at the same time, wherein 50 mL of the solution A contains 0.020 g of a heteropolyacid salt (NH4) 3 [CrMo6O24H6].7H2O, and 50 mL of the solution B contains 0.005 g of a (DABCO.2HBF4) salt; and (2) sucking 50mL of solution in the beaker after finishing dropping, repeating the step (1), and standing for 5 days to obtain the purplerodlike polyacid supramolecular crystal material. According to the invention, a better crystal material is grown by a double-component dropping method, and meanwhile, different quantities of crystalscan be obtained by controlling the dropping speed, and even a nanoscale crystal material can be prepared; the polyacid supramolecular crystal material prepared by the method can be widely applied tothe aspects of information storage materials, dielectric materials, polyacid catalytic materials, novel electrode materials, energy storage materials and the like.

The invention discloses synthesis and preparation of a series of pillared metal organic framework materials and application of the pillared metal organic framework materials in low-carbon hydrocarbon separation, and belongs to the technical field of crystalline porous material preparation and gas separation. The D-camphoric acid series pillared microporous MOF material is formed by cheap and easily available organic ligand D-camphoric acid (cam) and columnar ligands pyrazine (pyz), 2-aminopyrazine (apyz), triethylene diamine (dabco) and metal copper salt, cobalt salt and nickel salt under solvothermal conditions. The MOF crystal structure has high porosity and also has a regular pore channel structure, the channel size is slightly larger than the dynamic size of low-carbon hydrocarbon molecules, a structural basis is provided for low-carbon hydrocarbon gas molecule adsorption separation, and the MOF material is applied to efficient adsorption separation of ethane/ethylene mixed gas. The ethane gas molecules and the framework have stronger acting force, so that the effect of preferentially adsorbing the ethane gas in the ethane-ethylene mixed gas is realized, the ethylene component in the mixed gas is purified, and the energy consumption is reduced.

A method for increasing the rate of polymerization of 2-octyl cyanoacrylate, or the rate of copolymerization of 2-octyl cyanoacrylate and a tri-telechelic star polymer comprising polyisobutylene terminated with cyanoacrylate groups (Ø(PIB-CA)₃) to form a co-network, is provided. The method comprise initiating the polymerization of 2-octyl cyanoacrylate, or the copolymerization of 2-octyl cyanoacrylate and a tri-telechelic star polymer comprising polyisobutylene terminated with cyanoacrylate groups (Ø(PIB-CA)₃) to form the co-network, with an initiator selected from the group consisting of cyclic tertiary aliphatic amines optionally dissolved in a non-aqueous solvent. The cyclic tertiary aliphatic amines are selected from the group consisting of azabicyclo[2.2.2]-octane (ABCO), and 1,4-diazabicyclo[2.2.2]-octane (DABCO).

The invention discloses a synthesis method of a beta-ketosulfone compound, and belongs to the technical field of chemical synthesis. According to the synthesis method, tetrafluoroborate diazonium salt, alkyne and DABCO. (SO2) 2 are subjected to an oxidation bifunctionalization reaction to prepare the beta-ketosulfone compound. The method comprises the following steps: adding DABCO.( SO2) 2, alkyneand tetrafluoroborate diazonium salt which are used as reactants and mesoporous carbon nitride, an organic solvent, water and oxygen which are used as catalysts into a reactor, and stirring for 6-10hours at room temperature under the irradiation of visible light. The method is mild in reaction condition, simple to operate and high in atom economy, and the catalysts can be recycled.