97results about How to "Reaction temperature" patented technology

The invention provides a synthetic method of rosuvastatin calcium, which is characterized in that a compound 6 and branched chain react under the action of 2,2,6,6,-tetramethylpiperidine and n-butyl lithium to generate a compound 7, the reaction temperature is increased to minus 30 DEG C and the aspects such as reaction solvent and reaction reagent are improved so that the total reaction route has the advantages of mild condition, low device requirement and suitability for industrial production. Meanwhile, another improved synthetic route of rosuvastatin calcium comprises the following steps: converting esters into acids, synthesizing esters again, and synthesizing the rosuvastatin calcium. The rosuvastatin calcium purity is as high as 99.8%.

The invention belongs to the technical field of preparation methods for polypeptide medicines, and particularly relates to a method for preparing bivalirudin. The method for preparing the bivalirudin comprises the following steps of: preparing a bivalirudin resin by a solid phase polypeptide synthesis method, performing acidolysis on the bivalirudin resin to obtain a bivalirudin crude product, and purifying the bivalirudin crude product to obtain a bivalirudin pure product, wherein the step of preparing the bivalirudin resin by the solid phase polypeptide synthesis method comprises the following substeps of: sequentially accessing the corresponding protection amino acid or fragments on an Fmoc-Leu-carrier resin by a solid phase coupling and synthesis method to obtain the bivalirudin resin, wherein the corresponding protection amino acid or fragments have the following sequences: R1-D-Phe-Pro-X-Y-Phe-Glu(OtBu)-Glu(OtBu)-Ile-Pro-Glu(OtBu)-Glu(OtBu)-Tyr(tBu)-Leu-resin, R1 is Fmoc, Boc or H; X is Arg(Pbf)-Pro; Y is Gly-Gly-Gly-Asn(R2)-Gly-Asp-(OtBu); and R2 is Trt or H. The purity of the product can reach above 99.5 percent.

The invention relates to a preparation method for a Fe3O4/SiO2 nanometer particle containing multiple magnetism cores, which comprises (1) dissolving Fe3O4, cetyltrimethyl ammonium (CTAB) and tetraethyl orthosilicate (TEOS) in solvent, obtaining mixed solution after ultrasonic processing, then adding polyvinylpyrrolidone powder, and evenly stirring to achieve spinning solution; (2) using the spinning osolution to perform electrostatic spinning to obtain nanometer fiber; and (3) placing the nanometer fiber in ethanol water, and forcefully stirring at the temperature of 20 DEG C to 40 DEG C to achieve the Fe3O4/SiO2 nanometer particle containing the multiple magnetism core. The preparation method is convenient in operation, moderate in reaction condition, low in cost of raw materials, easy in obtaining the raw materials, free of poison and pollution and good in biocompatibility. The Fe3O4/SiO2 nanometer particle contains multiple magnetism cores, has excellent magnetic property, is uniform in particle diameter, regular in shape, high in chemical stability and has the advantages of a general nanometer particle.

The invention provides a production process for preparing dichloropropanol by reactive distillation of glycerol. The production process comprises the following steps: the raw material glycerol containing a homogeneous catalyst is sent to a reactive rectification tower from the top after heat exchange, hydrogen chloride gas enters from the lower part of a rectification section of the tubular reactive rectification tower, and the raw material glycerol and countercurrent flow of the hydrogen chloride gas are subject to absorption and chlorination reaction by a packing layer at the temperature of 90-120 DEG C and the temperature of 0.001-0.1MPa (absolute pressure) and are rectified; omonochloropropylene glycol at the bottom of the tubular reactive rectification tower, glycerol and glycerol oligomer are sent to a heavy constituent separation tower for decompressing and recovering the monochloropropylene glycol and the glycerol is returned to the raw material glycerol; and product gas on the top of tubular reactive rectification tower is cooled by a heat exchanger to obtain the dichloropropanol which is sent to a cyclization working procedure, and tail gas is further washed with lye, and is discharged from by a vacuum pump.

The invention provides a method for treating dye waste water. The dye waste water subjected to catalytic oxidation in advance is subjected to anaerobic-aerobic treatment, and then the waste water subjected to anaerobic-aerobic treatment is subjected to activated carbon adsorption and then drained out. Due to the fact that the dye waste water has the characteristics of being high in salt content and COD concentration, part of COD loads are reduced by carrying out catalytic oxidation at the front end in advance, sanitary sewage diluting and anaerobic-aerobic treatment are carried in the middle to reduce COD of the waste water, meanwhile, the salt content is reduced, the anaerobic-aerobic biochemical process can be carried out, activated carbon adsorption is conducted, and sewage water treatment is completed. The method is simple, moderate in reaction condition, high in speed and easy to operate, and a catalyst adopted during pretreatment can be recycled. During the reaction, acidic conditions are not needed, the pH value does not need to be adjusted, and consumption of a large amount of acid is avoided. The treatment process is short, and treatment efficiency is high.

The invention belongs to the field of environmental water pollution abatement, and discloses a ZnIn2S4 nanosheet coated beta-Bi2O3 core-shell heterogeneous compound photocatalyst, as well as a preparation method and application thereof. According to the method, the ZnIn2S4 nanosheet coated beta-Bi2O3 core-shell heterogeneous compound photocatalyst is prepared by using ZnIn2S4 and synthetic beta-Bi2O3 monomer as raw materials through a simple self-aggregation effect. The binary ZnIn2S4/beta-Bi2O3 compound nano-photocatalyst can be applied to catalytic degradation of tetracycline hydrochloride and methyl orange under visible light, shows excellent photo-induced electron separation efficiency, and can be used for improving the visible light utilization and integral photocatalytic activity. The ZnIn2S4 nanosheet coated beta-Bi2O3 core-shell heterogeneous compound photocatalyst is prepared from nontoxic raw materials, has simple operation and mild reaction condition, accords with the concept of environment-friendly chemistry, and has a wide application prospect in the aspect of solving water environmental pollution.

The invention provides a method for whole-cell catalytic synthesis of 1-hydroxy-2-butanone and belongs to the technical field of bioengineering. A mutant library is constructed by fixed-point saturated mutation of formaldehyde lyase 482 amino acid, and an engineering strain containing formaldehyde lyase (FLS) is obtained by screening. Whole-cell catalytic synthesis of the 1-hydroxy-2-butanone is realized with the strain as whole cells and formaldehyde and n-propanal as raw materials. The strain can produce the 1-hydroxy-2-butanone from one molecule of formaldehyde and one molecule of propionaldehyde under the action of the FLS. The method can finish synthesis of the 1-hydroxy-2-butanone in only one step, the reaction condition is mild, the raw materials are wide and easy to obtain, and thecost is low.

The invention relates to an application of prussian blue nanoparticles in preparation of drugs for preventing, delaying or treating nervous system degenerative diseases. Researches find that the prussian blue nanoparticles have remarkable effects in the aspects of preventing, delaying or treating nervous system degenerative diseases. Cell level test results show that the prussian blue nanoparticles can reduce the ROS level in nerve cells stimulated by hydrogen peroxide and increase the proportion of living cells in the nerve cells stimulated by hydrogen peroxide; and animal level test resultsshow that the prussian blue nanoparticles can significantly reduce the expression level of oxidative stress markers in hippocampus of nervous system degenerative disease model mice, significantly improve the learning and memory ability of nervous system degenerative disease model mice, and improve dyskinesia. The preparation process of the prussian blue nanoparticles is simple, the macro production is easy, the reaction condition is mild, and the surface modification is easy.

The invention relates to a preparation method of 2,4-diethyl thioxanthone. The preparation method of the 2,4-diethyl thioxanthone is characterized by finally obtaining a product, i.e. the 2,4-diethyl thioxanthone, through the processes of condensation, extraction, washing, caustic washing, distillation, dissolution and crystallization, centrifugation, drying, and the like by taking o-diethylbenzene and dithio-salicylic acid as main raw materials and sulphuric acid, toluene, sodium carbonate, methanol, and the like as auxiliary raw materials. The preparation method of the 2,4-diethyl thioxanthone, which is disclosed by the invention, has the advantages of higher yield reaching 85 percent through experimental determination, little acid pollution, easy aftertreatment, moderate reaction condition and capability of reducing the energy consumption because the distillation is not needed by the aftertreatment of the product.

The invention discloses a preparation method of cis-hexahydroisoindoline, which comprises the following steps: enabling maleic anhydride and 1,3-butadiene, which are used as raw materials, to be subjected to Diels-Alder reaction to obtain cis-1,2,3,6-tetrahydrophthalic anhydride (I); carrying out Pb/C hydrogenation on the product I to obtain cis-cyclohexanedicarboxylic anhydride (II); reacting the product II with carbamide to obtain cis-hexahydrophthalimide (III); and reducing the product III with lithium aluminum hydride in anhydrous tetrahydrofuran to obtain the target product cis-hexahydroisoindoline. The Mitiglinide calcium preparation method disclosed by the invention can save the raw material cis-hexahydroisoindoline, and has high chiral degree of separation.

The invention discloses titanium dioxide/baffeta with super-hydrophobic and self-cleaning functions. The titanium dioxide/baffeta is prepared by the steps of in-situ generating nanometer TiO2 particles in the baffeta, and cladding the TiO2 particles in the middle of BSA to obtain BSA/TiO2/BSA modified baffeta; then soaking the BSA/TiO2/BSA modified baffeta into a fluoroalkyl silane ethanol solution with the volume fraction being 1 to 10 percent for 1 to 24h, and after finishing reaction, repeatedly cleaning through deionized water, and vacuum drying to obtain the titanium dioxide/baffeta withthe super-hydrophobic and self-cleaning functions. A preparation method provided by the invention has the advantages of simplicity in operation, moderate reaction conditions and the like; the baffetahas an excellent super-hydrophobic performance, an excellent self-cleaning performance, an excellent anti-microbial performance, an excellent uvioresistant performance, an excellent photocatalysis performance, an excellent anti-wrinkle performance and excellent washing resistance.

The present invention discloses a difluoropropargyl-containing compound, a preparation method and applications. The preparation method comprises that in the presence of an organic solvent, a catalyst, a ligand and an alkali, a compound A and a compound B are subjected to a coupling reaction to obtain a compound C, wherein the catalyst is one or a plurality of materials selected from palladium acetate, palladium trifluoroacetate, tetrakis(triphenylphosphine)palladium, tris(dibenzylideneacetone)dipalladium chloroform adduct, and tris(dibenzylideneacetone)dipalladium, and the ligand is one or a plurality of materials selected from triphenylphosphine, tris(o-methoxyphenyl)phosphine, tris(o-methylphenyl)phosphine, tri-tert-butylphosphine fluoroborate, 2-(dicyclohexylphosphino)-2'-methylbiphenyl, 2-(di-tert-butylphosphino)biphenyl, and 4,5-bisdiphenylphosphino-9,9-dimethyl xanthene. According to the present invention, the method has characteristics of low catalyst consumption, mild reaction condition, high region selectivity, wide application range, and high reaction yield, and is suitable for industrial production. The compounds A, B and C are defined in the specification.

The invention provides optical fiber sensing equipment detecting oil-water interface of a storage pot and relates to the technical field of oil field measuring. Oil-water liquid surface can be monitored in real-time and with accuracy by monitoring of various temperatures of different medium layers such as air, an oil layer, an emulsion layer and a water layer of the oil storage pot. The optical fiber sensing equipment detecting oil-water interface of the storage pot comprises a ripple pipe vertically disposed in the oil storage pot. The bottom of the ripple pipe is provided with a horizontal base seat; an armored temperature measuring optical fiber winds the ripple pipe; the armored temperature measuring optical fiber at least comprises two multi-mode temperature-sensing optical fibers backing up for each other; the optical fiber sensing equipment further comprises a temperature sensor and a distributing optical fiber host; and the temperature sensor is connected with the distributing optical fiber host via the multi-mode temperature-sensing optical fibers.

The invention discloses a organic small molecule containing a boron-nitrogen coordination bond, and a preparation method and sensing application thereof to a fluorine ion, and belongs to the technicalfield of preparation of fluorescent compounds and preparation of fluorescent probes. According to the invention, 2-(3-bromobenzothiophen-2-yl)benzothiazole reacts with n-butyl lithium to form a lithium reagent, and then the lithium reagent reacts with triphenylboron to prepare the small molecule containing the boron-nitrogen coordination bond. Experiments verify that the small molecule containingthe boron-nitrogen (BN) coordination bond prepared by the invention can successfully realize selective recognition of the fluorine ion. The preparation method of the fluorescent compound containing the boron-nitrogen (BN) coordination bond of the invention is simple and convenient, the reaction condition is mild, and a prepared fluorescent probe has the characteristics of photochemical stabilityand good selectivity.

The invention provides cooling agent spice menthyl formate for a cigarette. A chemical formula of the cooling agent spice is as shown in the specification. The invention further provides a preparation method and an application of the cooling agent spice for the cigarette. The preparation method comprises the steps of mixing menthyl-3-carboxylic acid and thionyl chloride, conducting a backflow reaction till menthyl-3-carboxylic acid reacts completely, removing excessive thionyl chloride, adding anhydrous pyridine and menthol, reacting for 1-4h at 40-80 DEG C, separating and purifying after the reaction, and obtaining cooling agent spice menthyl formate for the cigarette. The cooling agent spice for the cigarette has obvious effects on improving the harmony and the softness of smoke of the cigarette, and reducing the irritation of an oral cavity and a throat, and is good in taste; the fragrance is similar to that of L-menthol, but is lasting; in addition, the cooling agent spice for the cigarette is simple in preparation process, mild and safe in reaction condition, and high in practicability; industrial production is facilitated; and the production cost of the cigarette cannot be increased.

The invention relates to field of organic synthesis, and aims to provide a method preparing N-aryl and N-alkyl aromatic amine type compound from phenol type compound. The method includes that the phenol type compound and ammoniation reagents are solved in organic solvent or mixed solvent of the organic solvent and cosolvent, alkali is added, reaction is conducted for 2-4 hours under 50-80 DEG C, temperature rises to 100-160 DEG C, stirring reaction is conducted for 2-24 hours, and aromatic primary amine type compound is obtained after postprocessing. Alternatively, part of alkali is added, reaction is conducted for 2-24 hours under 50-80 DEG C, another part of alkali is additionally added, temperature rises to 100-160 DEG C, stirring reaction is conducted for 2-24 hours, and the N-aryl and N-alkyl aromatic amine type compound is obtained after postprocessing. The method is wide in application range, strong in generality, high in yield, and simple and convenient to operate.

The invention discloses 5-alkyl guanidine ionic liquid, and preparation and application thereof. After tetramethyl guanidine and alkyl halide are adopted to be ionized, ion exchange with metal salt is performed to prepare 5-alkyl guanidine acid radical ionic liquid, and the ionic liquid is used as a catalyst to synthesize quinazoline-2,4(1H,3H)-ketone and derivatives thereof in the carboxylation and cyclization reaction of carbon dioxide and anthranilonitrile. Compared with the prior art, the 5-alkyl guanidine ionic liquid is simple in synthetic process, low in costs and has excellent performance in a homogeneous catalysis carbon dioxide reaction process; particularly, when the 5-alkyl guanidine ionic liquid is used in the carboxylation and cyclization reaction synthesis of the carbon dioxide and the anthranilonitrile, quinazoline-2,4(1H,3H)-diketone and derivatives thereof can be obtained in a relatively mild condition; the catalytic performance is good; the reaction condition is mild; and the postprocessing is easy. Meanwhile, the 5-alkyl guanidine ionic liquid can be used as a solvent and a catalyst; the use of a large quantity of organic solvent is avoided; and the 5-alkyl guanidine ionic liquid has important significance on researching medicinal chemistry and compounds of medical intermediates.

The invention provides a preparation method of NH4Fe1-xMxPO4 and LiFe1-xMxPO4/C materials. The preparation method of the LiFe1-xMxPO4/C material includes preparing a phosphorus source compound, a ferrous iron compound, a bivalent M metallic salt compound (M=Ni, Co and Mn) and a reducing agent into a mixture water solution, enabling the mixture water solution to react with an ammonia water solution to synthesize a sheet-shaped NH4Fe1-xMxPO4 precursor, and performing lithium doping and high-temperature heat treatment to obtain the LiFe1-xMxPO4/C material. The LiFe1-xMxPO4/C material prepared according to the preparation method has the advantages of high energy density, good cycle performance and high rate capability and is suitable for the application field of lithium-ion power batteries. The preparation method has the advantages of simple steps, convenience in operation and high practicality.