63results about How to "Use less solvent" patented technology

The invention provides an industrialized production method for high-purity decitabine. The method comprises the following steps of: 1, performing silanization reaction of 5-azacytosine, bis(trimethylsilyl)amine and trimethyl chlorosilane, which serve as raw materials, to prepare 2,4-bis(trimethylsilyl)-5-azacytosine; 2, performing reaction of the product obtained by the step 1 and 1-chloro-3,5-bis-(4-chlorobenzoyl)-2-deoxy-D-ribofuranose, which serve as raw materials, to prepare a crude product of 1-(3,5-bis-(4-chlorobenzoyl)-2-deoxy-beta-D-ribofuranose)-5-azacytosine; 3, dissolving the product obtained by the step 2 in a C5 to C7 hydrocarbon, stirring, filtering and drying to obtain a refined product; and 4, producing the high-purity decitabine by using the product obtained by the step 3, methyl alcohol and sodium methoxide as raw materials. The method overcomes the disadvantages of need of column purification, low purity, difficult industrial production in the prior art, and has the advantages of simple and convenient operation, small solvent consumption, small influence on the environment, low labor intensity, short period, high product purity, single impurity and less than 0.1 percent total impurity content.

The present invention is the preparation process of one-dimensional nanometer magnetic metal and alloy material, and relates to functional information material and biomedical material. The one-dimensional nanometer magnetic metal and alloy array material is prepared through utilizing porous polycarbonate or aluminan as template, regulating the metal ion concentration in electric deposited fluid, controlling the pH value and voltage of the depositing solution, assembling metal atoms into the processed template holes to form tubular or columnar structure, dissolving the template and centrifugally washing. Controlling the concentration of metal ions in the solution and other deposition factors can obtain two-component or multi-component alloy with different atom ratio. The prepared material has hollow structure and excellent soft magnetic performance and may be used in information storing and directional medicine releasing.

The invention discloses ZIF-8@SiO2 core-shell spheres. The ZIF-8@SiO2 core-shell spheres are composite microspheres having a core-shell structure in which SiO2 microspheres are taken as cores while ZIF-8 is taken as shells. The invention further provides a corresponding preparation method. The preparation method comprises the following steps: modifying SiO2 microspheres serving as cores with carboxyl to obtain SiO2-COOH; and then growing a zeolitic metal organic framework ZIF-8 shell layer on the surface layer by layer with a layer-by-layer alternative growth method. As proved by experiments,the composite microspheres have the characteristics of controllable coating thickness, regular appearance and high stability. The composite microspheres can be taken as a solid extraction material forpreparing an online solid extraction column, can be combined with high performance liquid chromatography for online enrichment detection of quinolone medicaments, has high repeatability and batch reproducibility, has high enriching performance for the quinolone medicaments, has the advantages of easiness, rapidness and efficiency in operation and small solvent dosage, and has a wide practical application prospect.

The invention relates to a preparation device for water-soluble nanometer material supercritical carbon dioxide anti-solvent, comprising a high-pressure pump for carbon dioxide, a high-pressure pump for solution, a nozzle, a crystallization reactor, a whole filtration membrane crystallizer, a separation reactor, and a cyclone separator, which is characterized in that: the nozzle and the whole filtration membrane crystallizer are arranged in the crystallization reactor, the aperture of the nozzle outlet is 1 to 1000um, the aperture of the whole filtration membrane crystallizer is 50 to 500nm, the cyclone separator is connected with the whole filtration membrane crystallizer arranged in the crystallization reactor, thus forming a closed recovery system for products. The preparation device has the advantages of large whole filtration membrane crystallizer area, fast crystallization, small particle size, uniform distribution, high crystallization rate of more than 80 percent, automatic collection of products without opening the cover of the crystallization reactor, ability to conversely blow the whole filtration membrane crystallizer utilizing carbon dioxide, and closely select products through the cyclone separator, thorough collection of products, rapid recovery of filter membrane flux, no pollution to environment, not harm to human body, less solvent consumption, high separation efficiency, fast speed, short cycle, low energy consumption, and easy operation.

The invention provides a method for extracting O-methyl nandinine from Nandina domestica, which mainly solves the problems of complex operation, low product content, low recovery rate and inadaptability to mass production operation in the prior art. The method comprises the following steps: 1] primary extraction; 2] secondary extraction; 3] cationic resin adsorption purification; and 4] anionic resin adsorption decolorization. The method can be utilized to obtain the O-methyl nandinine product with the purity of greater than 98% only by several steps, and is convenient to operate. The method has the advantages of high product content, high recovery rate and small solvent hazard, and is suitable for mass production operation.

The invention discloses a method for synthesizing pretilachlor. The method for synthesizing the pretilachlor sequentially comprises the following steps of: synthesizing N-(1-methyl-2-hydroxy ethyl)-2,6-diethylaminobenzene; synthesizing 2-ethyl-6-methyl-N-(1'-methoxyl-propyl-2-group)phenylamine; and synthesizing the pretilachlor and the like. The method is simple and practical and high in efficiency; yield of products in each step is over 92 percent; in the synthetic process, the adopted reagent has low toxicity, few solvents are used and few side reactions are generated, so corrosivity to equipment is low and environmental friendliness is achieved; and the raw materials are low in price, so the production cost is reduced, economical efficiency is high, and a good application prospect is achieved.

A negative-pressure chromatographic equipment is composed of cylindrical main body, the quick-unlocked locking top conic closure head with negative pressure port connected to negative pressure pump via valve and vapour-liquid separator, conic top fastener for said conic top closure head, the quickly-unlocked locking bottom conic closure head with liquid inlet connected to liquid outlet of three-way value via liquid inlet tube, and conic bottom fastener for said conic bottom closure head. Its advantages are high separation efficiency and speed, less consumption of solvent and energy, and no noise and pollution.

The invention discloses a molecularly-imprinted nanoparticle for glycoprotein and a synthesis method thereof, belongs to the field of analytical chemistry, and relates to synthesis of molecularly-imprinted polymers. The synthesis method comprises the following steps: firstly, preparing a solution phase A from template glycoprotein molecules, preparing a solution phase B from a functional monomer and a cross-linking agent, and preparing solution phase C from an initiator; secondly, respectively fixing the solution phase A, the solution phase B and the solution phase C on three micro-fluidic injection pumps with adjustable flow rates, connecting and mixing the solution phase A and the solution phase B through a Y-shaped three-way valve, connecting and mixing the mixed solution and the solution phase C through another Y-shaped three-way valve, and enabling the obtained mixed solution and the solution phase C to flow into a reactor for a polymerization reaction; and finally, collecting a polymerized nanoparticle at the tail end of the reactor, and removing the glycoprotein template molecules to obtain the molecularly-imprinted nanoparticle for glycoprotein. The molecularly-imprinted nanoparticle for glycoprotein is prepared in a microfluidic mode, operation is easy, continuous production can be achieved, and the obtained molecularly-imprinted nanoparticle can be used for specific recognition of target glycoprotein molecules.

The invention relates to the field of synthesis of medicines, in particular to a minodronate crystalform II and a preparation method thereof. The minodronate crystalform II is characterized in that an X-ray powder diffraction pattern has characteristic peaks when a reflection angle 2theta is close to 10.32, 11.16, 13.14, 15.02, 15.72, 17.44, 20.28, 20.72, 21.46, 22.30, 23.48, 25.64, 26.48, 28.80, 30.14, 32.30, 34.58, 35.50 and 36.34. The minodronate crystalform II has high solubility and dissolution rate.

The invention relates to a preparation method of amorphous dasatinib, wherein the preparation method includes the steps: dissolving raw materials of various crystal types of dasatinib in an anhydrous organic solvent at the temperature of 60-100 DEG C, adding a cosolvent for helping dissolution, and thus obtaining a fully-dissolved dasatinib solution; carrying out spray drying on the dasatinib solution, carrying out cyclone isolation, and rapidly precipitating to obtain a dasatinib solid powder; drying the dasatinib solid powder under reduced pressure, removing the solvent, and thus obtaining the dasatinib amorphous product. Through testing, the prepared amorphous dasatinib has the moisture content generally less than 2%, and is nearly anhydrous dasatinib. The method is suitable for converting various crystal types of dasatinib into the dasatinib amorphous product having the residual solvent consistent with Chinese pharmacopoeia, and the preparation yield reaches up to more than 99%. Moreover, the method has the advantages of simple operation, less operation steps, less using solvent, small process pollution, low cost and the like, and is suitable for large-scale industrialized production.

The invention provides a method for extracting polyphenolic compounds from seabuckthorn fruit. According to the invention, seabuckthorn dried fruit powder or dry seabuckthorn fruit pomace are well mixed with diatomite, and the mixture is subjected to extraction in an extraction tank; filtering is carried out after extraction is finished, such that an extraction liquid is obtained; the liquid is concentrated and lyophilized, such that polyphenolic compounds in seabuckthorn fruit are obtained. The method provided by the invention has the advantages of short extraction time, low solvent dosage, and high extraction efficiency.

The invention discloses a nickel metal complex as well as a preparation method and an application thereof. The structural formula of the nickel metal complex is shown as a formula (III), wherein R isethyl, isopropyl or cyclohexyl in the formula (III). The nickel metal complex prepared by the preparation method disclosed by the invention is applied to the process of preparing the K-type perfluoropolyether oil as a catalyst and can effectively prepare the K-type perfluoropolyether oil with high polymerization degree, improves the product yield and reduces the amount of used solvents and the like, thereby effectively promoting the reduction of the production cost of the K-type perfluoropolyether.

The invention discloses a preparation method of high-purity monoacetyl ganciclovir. The method comprises the steps of taking ganciclovir as a raw material; protecting an alcoholic hydroxyl group through sulfite; then adding an acetylation agent to perform selective acetylation, thus obtaining the monoacetyl ganciclovir. The method is high in raw material conversion rate, and high in acetylation selectivity; the content of the obtained monoacetyl ganciclovir reaches 99% or higher, thus the synthesizing quality of following valganciclovir products can be improved; the production efficiency is high; the method is suitable for massive industrial production.

The invention discloses a detection method of a genotoxic impurity diisopropyl sulfate in a medicine. The detection method comprises dissolving a thymol drug raw material, carrying out extraction, carrying out centrifugal separation at a high speed to obtain a supernatant, and analyzing the supernatant through a triple tandem quadrupole high-performance liquid chromatography-mass spectrometer to detect the content of the genotoxic impurity diisopropyl sulfate in the thymol drug raw material. According to the detection method, a diisopropyl sulfate recovery rate is in a range of 90-110%, a standard deviation (RSD) is 2.33%, a detection limit is 1.74 micrograms/kilogram and a quantitation limit is 5.81 micrograms/kilogram. The method has a low detection limit, a high recovery rate, high sensitivity and good repeatability and can be used for detection of genotoxic impurity diisopropyl sulfate in pharmaceutical raw materials including drugs difficult to gasify.

The invention discloses a preparation method of label ink resistant to yellowing at 300 DEG C continuously and used for a PI (polyimide) base material. The preparation method comprises following steps: (1), resin, a dispersing agent, a dispersing solvent, a modifier and a stabilizer are stirred uniformly at a low speed, pigment and filler are added in sequence, the components are stirred uniformlyat a high speed, and a dispersed material is obtained, wherein the resin is saturated polyester and the filler is inorganic micro-powder; (2), the dispersed material is ground, and a main agent is obtained; (3), the main agent is mixed with a curing agent and a diluent, and the label ink resistant to yellowing at 300 DEG C continuously and used for the PI base material is obtained. Multiple problems about adhesive force, ribbon printing performance, yellowing resistance at 300 DEG C for 60 min and the like are solved while the cost is greatly reduced, the unexpected technical effect is realized, and the label ink can perfectly replace the same foreign imported products.

The invention provides a method for detecting related substances of palonosetron hydrochloride injection, which comprises the steps of enriching the palonosetron hydrochloride injection by adopting asolid phase extraction cartridge, eluting, and performing liquid chromatography analysis under the conditions that: chromatographic column: the filler is bonded vancomycin; detection wavelength: 235 to 245 nm; column temperature: 30-40 DEG C; flow rate: 1.4-1.6 mL/min; mobile phase: ammonium acetate solution and tetrahydrofuran mixed solution. The related substances of the palonosetron hydrochloride enriched by the method can be concentrated by more than 10 times, the influence of auxiliary materials can be removed at the same time, one-time extraction and detection of fat-soluble and water-soluble impurities in a sample can be realized, the related substances can be accurately detected, therefore, the method is high in sensitivity, simple and convenient to operate and accurate in result.