119results about How to "Novel synthetic method" patented technology

The invention discloses a 4, 5-disubstituted-2-aminothiazole compound. The structural formula is shown in the specification, wherein R1 is 4-tolyl, 4-chlorophenyl, 4-methoxyphenyl, 4-nitrobenzene or propoxy, and R2 is phenyl, 4-tolyl, 4-fluorophenyl, 4-methoxyphenyl, 2-furyl, isopropyl, 4-nitrophenyl or n-propyl. The invention simultaneously provides a preparation method of the 4, 5-disubstituted-2-aminothiazole compound. The preparation method comprises the following steps: enabling an olefin azide type compound and potassium thiocyanate to react at the temperature of 75-85 DEG C in the presence of a solvent and a metal catalyst, concentrating an obtained reaction solution, then extracting with water and ethyl acetate, washing an obtained organic layer, then drying and concentrating by a rotary evaporator; performing silica gel column chromatography on an obtained concentrate to obtain the 4, 5-disubstituted-2-aminothiazole compound.

The invention belongs to the technical fields of medicaments and organic synthetic intermediates and in particular relates to a method for synthesizing 4-aryl-1H-1,2,3-triazole by using 1,1-dibromo-1-olefin. A 4-aryl-1,2,3-triazole compound is synthesized by using a sodium azide or organic nitrine compound and cheap and readily-available 1,1-dibromo-1-olefin as raw materials in the presence of alkali in dimethylsulfoxide through copper catalysis conveniently. The compound comprises a 1,2,3-triazole structure unit with bioactivity and can be used for synthesizing and modifying the organic synthetic intermediates and the medicaments. A novel and effective synthetic method is provided for medicament screening.

The invention relates to a new method for preparing crystalline transitional metal boride CoB (cobalt boride) with oxide or hydroxide of cobalt and borohydride of cobalt through solid phase reaction. The method provided by the invention comprises the steps as follows: uniformly mixing oxide or hydroxide of cobalt and borohydride of cobalt according to the molar ratio of 1:1 to 1:1.5, tabletting under the pressure of 15 to 20 MPa, keeping the temperature of 400 to 800 DEG C for 6 to 24 hours under the protection of argon gas, and cooling to the ambient temperature slowly; and the obtained product is washed fully with deionized water and alcohol and then vacuum dried, thus the product CoB can be obtained. The method has the characteristics that the synthetic method is novel, the adopted process is simple, and pure crystalline CoB can be obtained without high temperature, high pressure or other complicated procedures; and the used raw materials are simple and easy to obtain, and the cost is low, so that the method is applicable to mass production.

The invention discloses the reduction-state ionic salt of perylene bisimide and a derivative thereof as well as a preparation method. The preparation method comprises the following steps: with perylene-3,4,9,10-tetracarboxylic acid dianhydride as a raw material, synthesizing a perylene bisimide derivative with low LUMO energy level and excellent photoelectric performance through a bromination reaction, an amidation reaction and a nucleophilic substitution reaction; and synthesizing the perylene bisimide monovalent ionic salt with stable environment relatively easily according to the benzoquinone type transformation mechanism in an alkaline condition (organic base such as triethylamine, and inorganic base such as potassium carbonate). The method for synthesizing the perylene bisimide ionic salt is novel, unique and simple and realizes high yield; industrialization can be implemented while the effect is good; and moreover, the material in a reduction state responds to metal ions and acids different in oxidability.

The invention discloses an ultraviolet light-cured biomass epoxy acrylate prepolymer and a synthesizing method and application thereof. The synthesizing method comprises the following steps of using cardanol as a main raw material, enabling phenolic hydroxyl in cardonol molecules and epichlorohydrin to react, enabling double bonds in the cardonol molecules and hydrogen peroxide to react so as to lead in a plurality of epoxy groups, and then reacting with (methyl)acrylic acid, so as to synthesize the ultraviolet light-cured biomass epoxy acrylate prepolymer. The synthesizing method has the advantages that the method is novel, the operation is simple, and the repeatability is good; the synthesized biomass epoxy acrylate prepolymer contains a cardanol group, so that a product has better hydrophobic property and chemical reagent-resistant property, the viscosity and rigidity of the product are correspondingly improved, and the prepolymer can be applied to the fields of ultraviolet light-cured coatings, ink, adhesives and the like.

The present invention is the preparation process of 3, 3', 5, 5'-tetralkyl-4, 4'-diphenol, and features that material 2, 6-dialkyl phenol is first oxidized and coupled with salt oxidant to produce 3, 3', 5, 5'-tetralkyl-4, 4'-biphenyl diquinone, and 3, 3', 5, 5'-tetralkyl-4, 4'-biphenyl diquinone is then reduced with cheap efficient inorganic reductant to obtain 3, 3', 5, 5'-tetralkyl-4, 4'-diphenol. The preparation process of the present invention is novel, mild in reaction condition, less in side product, simple and low in cost, has no need of blowing in oxygen or pressurizing air and special reaction apparatus, and has industrial application foreground.

The invention discloses a preparation method of a cuprous oxide nano material and hydrogen evolution performance of the cuprous oxide nano material, and belongs to the technical field of nanometer materials. According to the preparation method, ethylene glycol and diethylene glycol are used as reducing agents, copper hydroxide and basic copper carbonate with specific morphology are used as coppersources, and the copper hydroxide and the basic copper carbonate copper are reduced to form cuprous oxide nano material with maintained morphology under the protection of inert gas through a gas phasereduction method. The reaction steps are simple and are environmentally friendly, the obtained product does not need to be washed, and a pure cuprous oxide product can be obtained. According to the preparation method provided by the invention, the simple and rapid method is adopted for synthesizing the cuprous oxide nano material with the maintained morphology, and the prepared cuprous oxide nanomaterial has the performance of electro-catalytic hydrogen evolution.

The invention discloses production of an all-polymer self-supporting electrode and an application of the all-polymer self-supporting electrode in a flexible electrochemical sensor, and relates to thetechnical field of electrochemical sensors. The production comprises the following steps: a) producing a polypyrrole film with a sandwich structural formula by adopting an electrochemical polymerization method; and synthesizing a pentaerythritol ethoxylate- polypyrrole (PEE-PPy) film by adopting an electrochemical polymerization mode in an organic phase system, namely an organic electrolyte, taking a glass sheet plated with titanium and platinum in sequence as a working electrode, taking a stainless steel electrode as a counter electrode, and taking a silver wire as a reference electrode; According to the production of the all-polymer self-supporting electrode and the application of the all-polymer self-supporting electrode in the flexible electrochemical sensor, the polypyrrole compositefilm with the sandwich structural formula is used as the self-supporting electrode for detecting dopamine by the flexible electrochemical sensor, and the sensor does not need to be assembled by combining an additional current collector, a mechanical substrate, a conductive additive and the like; and dopamine detection sensitivity is high, the stability is high, and the capability of bearing long-term mechanical deformation is realized.

The invention belongs to technical field of pharmaceuticals and organic synthesis intermediates, particularly relates to a method for synthesizing 1-substituted-1, 2, 3-triazole from sodium acetylide. The specific procedure comprises the following steps: adding dimethyl sulfoxide (DMSO), organic azide and sodium acetylide into a reactor, reacting at room temperature under magnetic stirring for 1-30 min, diluting reaction system with water after reaction, performing extraction with ethyl acetate, washing the organic layer with saturated saline and drying with anhydrous sodium sulfate, evaporating out solvent under reduced pressure to obtain crude product, and purifying with column chromatography with ethyl acetate/petroleum ether as eluent to obtain product, wherein the molar ratio of sodium acetylide to organic azide is (3.5-15):1, the molar ratio of DMSO to organic azide is (20-500):1, and the volume ratio of ethyl acetate to petroleum ether in the eluent is 1:20-4:1. The obtained compound contains 1, 2, 3-triazole structure unit with physiological activity, and can be used as organic synthesis intermediate and for synthesis and modification of pharmaceuticals. The invention also provides a novel and efficient synthesis method for drug screening.

The invention discloses a method for synthesizing acetanilide derivatives, and belongs to the technical field of organic synthetic intermediates. The method particularly includes steps of adding aniline derivatives, potassium thioacetate, tert-butyl nitrite and acetonitrile into reaction tubes; tightening plugs of the reaction tubes; carrying out magnetic stirring reaction at the temperature of 25DEG C for 4 hours. The aniline derivatives and the potassium thioacetate which is low in cost and easy to operate, is easily available and is stable are used as acetylation reagents, and accordinglya series of acetanilide derivatives can be efficiently synthesized by the aid of the method under the room-temperature conditions. The acetanilide derivatives which are compounds contain arylamine skeletons and can be used for synthesizing and modifying organic synthetic intermediates and medicines, and novel and effective synthesis processes can be provided to screening medicines. The reaction can be accelerated by the tert-butyl nitrite to synthesize the compounds which are the acetanilide derivatives. Compared with existing synthesis methods, the method has the advantages that reaction conditions are simple, raw materials for the acetanilide derivatives are low in cost and easy to operate, are easily available and are stable, and functional groups of substrates are good in tolerance.

The invention discloses a method for preparing a two-dimensional Fe3O4 nano material. The method comprises the following steps of A, preparing an egg white solvent; B, preparing the two-dimensional Fe3O4 nano material; and C, washing. Compared with the prior art, the method has the advantages that the synthetic method of the Fe3O4 nano material is simple and novel, can be accomplished by one step, is easily operated and high in repeatability; the two-dimensional profile of the material can be controlled under the condition that egg white is used; the size in the same dimension can be controlled; and the method can be widely used for preparing other two-dimensional metallic oxides. Besides, products prepared by the method have the characteristics of high purity, uniform size distribution and the like.

The invention discloses an autocatalytic antibacterial agent of a polysaccharide-based nanodot aggregate and a preparation method and application of the autocatalytic antibacterial agent, belongs to the technical field of antibacterial nanotechnology, and relates to an antibacterial agent as well as a preparation method and application of the antibacterial agent. The invention aims to solve the problems of poor antibacterial effect and large side effect caused by low permeability of the existing nano antibacterial agent to a bacterial biofilm. The autocatalytic antibacterial agent of the polysaccharide-based nanodot aggregate releases Cu < 2 + > and H2O2 under acidic conditions, generates Fenton reaction to generate. OH with catalytic activity, and does not release Cu < 2 + > and H2O2 under neutral or alkaline conditions. The method comprises the following steps: 1, preparing a glucan/CuCl2 solution; 2, adding a NaOH solution and a H2O2 solution, and carrying out a stirring reaction; 3, centrifugal cleaning. The autocatalytic antibacterial agent of the polysaccharide-based nanodot aggregate releases. . OH with catalytic activity under an acidic condition, and is used for killing bacteria, inhibiting the formation of a bacterial biofilm and removing the formed biofilm.

The invention relates to a preparation method of p-toluene sulfonic acid quaternary amine of carboxymethyl chitosan, which is characterized by comprising the following steps of: under the protection of nitrogen, adding potassium carbonate, acetonitrile and methyl p-toluene sulfonic acid, controlling the temperature of 15 DEG C+3 DEG C, dripping acetonitrile solution of carboxymethyl chitosan, carrying out mechanical stirring for 5 minutes under room temperature, rising temperature to 83 DEG C, and carrying out violently backflow reaction for about 22 hours. The preparation method has the following advantages of having lower price and easy obtaining for reaction materials, mild reaction, simple condition, stability, easy production on scale and novel synthesis method, avoiding the use of highly toxic reagent of methyl iodide and dimethyl sulfate and the like, cleanness, environmental protection and greatly reducing hazard and toxicity; and the products has obvious leap in the properties of absorption and regeneration.

The invention relates to a carbon shell-coated lead molybdate nanocrystal and its preparation method. Citric acid is used to control synthesis of lead molybdate nanometer materials with different carbon shell thicknesses. Specifically, the preparation method is simple and novel and has strong controllability. The synthesized carbon layer-coated lead molybdate composite nanocrystal has high purity, and length and width of the nanocrystal are about 100 nm and 50 nm. In addition, the carbon shell coated outside the obtained lead molybdate composite material is more beneficial to separation and transfer of electrons. The carbon shell-coated lead molybdate nanocrystal is used as a cathode material for photoelectrocatalytic water-splitting, and stability and catalytic efficiency of the material also can be enhanced. The invention accords with researches on the latest clean energy and sustainable energy sources.

The invention discloses a coumarin-dithiocarbamate derivative and a synthesizing method thereof. The synthesizing method of the derivative comprises the following steps: 1) utilizing concentrated sulfuric acid as a catalyst, taking resorcinol and ethyl acetoacetate and putting into a first organic solvent to react to obtain an intermediate 2; 2) taking the intermediate 2 and dibromoalkane, puttinginto a second organic solvent and performing reaction under the condition that a pH is larger than or equal to 8 to obtain an intermediate 3; 3) taking the intermediate 3, carbon disulfide and secondary amine, putting into a third organic solvent and performing reaction under the condition that a pH is larger than or equal to 8 to obtain a corresponding target compound crude product. The synthesizing method disclosed by the invention has the advantages of simpleness and easiness in operation, high yield and stable quality; the synthesized coumarin-dithiocarbamate derivative has better acetylcholine esterase inhibiting activity; a lead compound is provided for developing novel AD treating medicine.

The invention discloses a preparation method of a 4, 5-disubstituted-2-aminothiazole compound. The preparation method sequentially includes following steps: 1), reacting a nitro epoxy compound, a hydrogen cyanamide water solution of 50% in mass concentration and sulfide in a solvent at room temperature; 2), concentrating reaction liquid obtained in the step 1) to remove the solvent, cooling to room temperature, using water and ethyl acetate to extract, and subjecting an obtained organic layer to washing, drying and concentrating by a rotary evaporator; 3), performing silica gel column chromatography on concentrate obtained in the step 2) to obtain the 4, 5-disubstituted-2-aminothiazole compound. A method which is simple and easy to implement is provided for efficiently synthesizing the 4, 5-disubstituted-2-aminothiazole compound.

The invention provides a preparation method of rare earth fluoride/poly-azobenzene/N-isopropyl acrylamide composite multifunctional nano-particles. The composite multifunctional nano-particle is provided with a yolk structure, and has the intelligent response characteristic due to the dual-responsiveness of a shell layer; the yolk structure enables the nano-particle has sufficient storage space, thereby realizing the effective load and controllable release of the anti-tumor medicine. The method comprises the following steps: 1) synthesis of homogeneous rare earth nuclear shell nano-particle; 2) cladding a silica layer with shell layer thickness of about 15nm through a reverse micro-emulsion method; 3) preparing dual-responsive shell by taking photo-responsive azobenzene as crosslinking agent and N-isopropyl acrylamide as the monomer; and 4) preparing the multifunctional nano-particle of the yolk structure with inner core as the rare earth nano-particle and the shell as the dual-responsive shell layer through a HF etching silica layer. The multifunctional rare earth nano-particle provided by the invention can be applied in the biological medicine field to a certain degree.

The invention relates to a synthesis method of stable isotope 18O labeled nipagin ester. The synthesis method comprises the following steps: taking stable isotope 18O-water as a raw material to reactwith benzoic acid-4-diazosulfate by utilizing different feeding amounts of the 18O-water; carrying out column chromatography silica gel separation to obtain an intermediate product p-hydroxy benzoic acid-18O or p-hydroxy benzoic acid-18O2 respectively; then enabling the intermediate product to be subjected to condensation reaction with a hydroxyl compound under the condition of a catalyst and an organic solvent; finally, separating and purifying to obtain a target product nipagin ester-18O or nipagin ester-18O2. According to the synthesis method provided by the invention, the prepared 18O labeled nipagin ester series product has the advantages that the chemical purity is higher than 98 percent and the abundance of stable isotopes is higher than 95 percent atom 18O; the product can sufficiently meet a mass spectrum detection internal standard substance for detecting content of nipagin ester type preservatives in foods and cosmetics.