150results about How to "Synthetic operation is simple" patented technology

The invention relates to a synthesis method for a visible photocatalyst by modifying titanium dioxide (TiO2) by using ammonium fluoride (NH4F). The synthesis method comprises three steps of: preparing a mesocellular foam silica (MCF) molecular sieve, preparing an MCF carrying TiO2 catalyst and modifying MCF / TiO2 by using the NH4F. Compared with the prior art, the carrying catalyst MCF / TiO2 is subjected to NH4F hydrophobic modification through a hydrothermal process and a low-temperature vacuum activation method; as a mesoporous material has extremely high absorption capability, the visible photocatalyst has outstanding absorption performance and catalyzing and degrading performance on ultraviolet and visible light of high-concentration organic pollutants during degrading of organic compounds, such as rhodamine B and the like; furthermore, during hydrophobic modification, if isopropyl alcohol is found to be a solvent, the NH4F hydrophobic modification effect of the prepared catalyst isthe optimal and the hydrophobic stability is quite good; moreover, the synthesis method is simple in operation and low in cost, and the raw materials are easily obtainable.

The invention relates to new benzocyclobutane, a preparation method thereof and application thereof. The invention provides a new preparation method for (1S)-4, 5-dimethoxy-1-(methyl-amino-methyl)-benzocyclobutane serving as a key intermediate of ivabradine hydrochloride and addition salt thereof, and meanwhile provides a new benzocyclobutane compound which is an intermediate for preparing the (1S)-4, 5-dimethoxy-1-(methyl-amino-methyl)-benzocyclobutane. In addition, the invention also provides a method for preparing the new benzocyclobutane compound, and meanwhile provides a method for splitting an intermediate product during preparing the new benzocyclobutane compound.

The invention discloses surface imprinting chitosan microspheres for efficiently selecting heavy-metal ions and a preparation method for the surface imprinting chitosan microspheres and belongs to the field of adsorbent synthesis. The preparation method comprises the steps of carrying out carboxylation modification on chitosan by adopting sodium chloroacetate so as to obtain electronegative carboxylated chitosan microspheres, then, carrying out surface adsorption by using a pre-assembled complex of polyethyleneimine and the heavy-metal ions, then, fixing imprinted sites by using epoxy chloropropane as a cross-linking agent, finally, eluting the heavy-metal ions by adopting an ethylenediamine tetraacetic acid solution, and carrying out freeze-drying, thereby obtaining the surface imprinting chitosan microspheres. The surface imprinting chitosan microspheres are simple in synthesis process, low in preparing cost and stable in surface imprinting hole spatial-configuration, thereby having a specific recognition function on template heavy-metal ions, and the high-selectively separated removal and resource recovery of the heavy-metal ions from wastewater can be realized, so that environmental and economic benefits are remarkable.

The invention discloses a novel peptide-link base-oligonucleotide compound and a solid phase gradual synthesis method thereof. The peptide-link base-oligonucleotide compound provided by the invention has the structure of a general formula (VIII), wherein X is a polypeptide structure part, A is substituted and unsubstituted benzene ring or carbon atom, and n is 0,1,2,3,4 or 5. The peptide conjugating oligonucleotide compound of the invention has the characteristics of simple structure, convenient synthesis and the like, the product has membrane permeability, can serve as a molecular biology tool for researching antisense oligonucleotide and small-interference RNA (siRNA) and has potential drug development prospect. The solid phase gradual synthesis method of the invention avoids difficult synthesis of the current biomacromolecule conjugate, simplifies synthesis operation, and is convenient to prepare the decorated oligonucleotide compound with high flux and multiple target spots.

The invention discloses an extraction method of active substances in mulberry leaves and a storage method of active substances in mulberry leaves. The extraction method of the active substances in mulberry leaves comprises the following steps of mixing a natural low-eutectic solvent with water so as to obtain an extraction solvent; adding mulberry leaves, and carrying out heated extraction at 60-90 DEG C for 0.5-3.0 hours; and carrying out centrifugation so as to obtain liquid supernatant, wherein the liquid supernatant contains active substances, including polyphenols, flavones, polysaccharides, alkaloid and the like. Moreover, the active substances are stored in the liquid supernatant containing the natural low-eutectic solvent so that stability of the active substances is greatly improved. According to the extraction method disclosed by the invention, the natural low-eutectic solvent of plant-source components is used as an extraction solvent and a stabilization assistant so as to be subjected to active substance extract; and thus, the extracted active substances are broad in spectrum, and the prepared product is natural and safe in property. Moreover, interaction between hydrogen bonds of the natural low-eutectic solvent is also utilized so as to improve stability of the active substances; and thus, the extraction method is significantly superior than the prior art.

The invention provides a preparation method and application of a nitrogen-doped porous carbon-coated cobalt nanoparticle composite material. The preparation method comprises the following steps: uniformly dispersing a carbon source precursor, a nitrogen source precursor and soluble salt of transition metal ions in a solvent according to a ratio, then performing drying to obtain a solid powder precursor, and calcining the solid powder precursor in a protective atmosphere to obtain black powder, namely the composite material. The composite material has efficient oxygen reduction catalysis performances and can be applied to proton exchange membrane fuel cells, alkaline fuel cells and metal-air batteries. The catalyst has the advantages that a pore structure is generated in the heat treatmentprocess and is uniformly dispersed; the carbon source, the nitrogen source and the metal source interact with one another to stabilize active elements and effectively improve the catalytic activity. Compared with a catalyst with commercial carbon as a carbon source, the prepared composite material has better oxygen reduction catalytic activity and is an efficient non-noble metal oxygen reduction catalyst.

The invention discloses a (+)-(3R,4R)-[[2S-[[4-(3-hydroxyphenyl-3,4- dimethyl-1-nipecotic)-methyl]-1-oxo-3-phenylpropyl]amido]benzyl cetate compound and its process for preparing and a new technology for preparation of Mope by the said compound. The new technique of this invention changes the íŒone chainíŒ synthesis of the original patent method to the separate í‹two chainsíŒ preparation, by which the total compound steps are dramatically shortened, the compound cost is reduced to about one-half of the original patent method, and the method is more competitive on the market in price. Furthermore,the reaction condition is moderate, the operating procedure is simple, each reaction step is no need of given condition such as low temperature and absolute water-free, so it is more suitable for industrial production.

The invention discloses a method for synthesizing a rivaroxaban intermediate 4-(4-aminophenyl)-3-molindone. The method comprises the following steps: reacting paranitroaniline with ethylene oxide to obtain a compound II; performing a cyclization reaction on the compound II and bromoacetyl bromide to obtain a compound III; adding the compound III into iron powder to perform a reduction reaction to obtain the 4-(4-aminophenyl)-3-molindone. According to the method, the raw materials are low in cost and easily obtained, the cost is low, the synthesis operation is simple, industrial nitration is avoided, environmental pollution is greatly reduced, and the method is suitable for industrial production.

The invention discloses a method for synthesizing dimethyl carbonate under the catalysis action of an ionic liquid. The bifunctional ionic liquid is adopted as a catalyst, a transesterification reaction is performed between ethylene carbonate and methanol, wherein when the use amount of the catalyst is 0.5-10 mol% of ethylene carbonate, the molar ratio of ethylene carbonate to methanol is 1:(5-30), the reaction temperature is 40-70 DEG C, and the reaction time is 2-12 h, so that dimethyl carbonate and ethylene glycol are synthesized with a high conversion rate and high selectivity. The methodhas the following advantages: (1) the bifunctional ionic liquid adopted as the catalyst has the effect of a homogeneous reaction and the characteristic of a heterogeneous catalyst, the shortcomings ofconventional solid catalysts and the homogeneous catalysts are overcome, and high catalytic activity, easy separation, recyclability and no pollution to the environment are achieved; (2) since the bifunctional ionic liquid is applied to the reaction system, reactants can be activated under the synergistic action of anions and cations of the catalyst, higher catalytic activity is achieved, and synthesis operation of the catalyst is simple and easy.

The invention discloses a water-phase preparation method of silicon quantum dots, comprising the following steps: (1) taking a reducing agent and a silane coupling agent and dissolving them in water under the protection of an inert gas, and the molar ratio of the silane coupling agent to the reducing agent is: 1:0.2~10; (2) Transfer the mixed solution obtained in step (1) into a high-pressure reactor and heat it to 140-220°C, and the silicon quantum dot solution can be obtained after the reaction; or the mixed solution obtained in step (1) The solution is transferred to a microwave reactor and heated to 140-220°C, and the silicon quantum dot solution can be obtained after the reaction; (3) the silicon quantum dot solution obtained in step (2) is mixed with an organic solvent, centrifuged, and the supernatant is removed. dry to obtain solid silicon quantum dots; wherein the reducing agent is citric acid, sodium sulfite, sodium borohydride, sodium citrate, ascorbic acid, urea, thiourea, hydrazine hydrate, L-cysteine, bovine serum albumin or Mixture of two or more in denatured bovine serum albumin.

The invention relates to a molecular sieve preparation technology, and aims at providing a method for synthesizing ZSM-48 zeolite through solvent-free solid-phase synthesis. The method comprises the following steps of using a silicon source, an aluminum source, ammonium fluoride and 4-dimethylamiopryidine used as a template agent into a mortar; performing grinding for 5 min; putting a mixture obtained after the grinding into a reaction kettle; performing crystallization reaction for 1 to 8d at 140 to 200 DEG C; after the reaction is completed, performing suction filtration and drying on the products to obtain the ZSM-48 zeolite. Compared with the prior art, the product obtained through preparation has the advantages that the good crystallinity and purity are maintained; good catalytic reaction activity is realized. No solvent is used in the whole production process; unnecessary loss in the production process is reduced; the yield is greatly improved. The synthesis operation is simple; the implementation is easy; the cost of using the expensive organic template agents is reduced; the important significance is realized in the practical chemical production field.

The invention discloses a sulfonated polybenzimidazole proton exchange membrane with the general molecular formula defined in the description, wherein polymer is random copolymer; n is greater than 0and smaller than or equal to 0.8; m is greater than or equal to 0.2 and smaller than 1; m+n is equal to 1; and the weight-average molecular weigh of the polymer is 5000-800000. The sulfonated polybenzimidazole proton exchange membrane has the advantage of high proton conduction rate.

The invention relates to a gasoline selective hydrogenation desulfurization catalyst, and a preparation method and application of the catalyst. The carrier of the catalyst is gamma-Al2O3 obtained through hydrothermal treatment, the specific surface area of the carrier is in a range of 70-140 m<2> / g, the pore volume of the carrier is in a range of 0.35-0.50 ml / g, and the active components of the carrier are cobalt and molybdenum. The preparation method of the catalyst comprises the following steps: performing hydrothermal treatment at a certain temperature on the gamma-Al2O3 obtained by roasting pseudo-boehmite; performing drying and roasting for re-dehydration to obtain a new gamma-Al2O3 carrier; performing dipping by using the active components molybdenum and cobalt, and performing dryingand roasting to obtain the catalyst. The catalyst provided by the invention has good gasoline hydrogenation desulfurization selectivity, the liquid yield is high (nearly 100%). the octane number lossis low (when the whole-fraction FCC gasoline is directly treated, and the content of the product S is about 10 ppm, the octane number loss is 2.1-2.3 units), and the catalyst has the advantages of simple preparation, low cost and the like.

The invention discloses a device and a method for generating person photograph materials. The device comprises terminal equipment. The terminal equipment comprises a photograph collection unit used for collecting person photographs from a local photograph album; a head portrait cut-out unit used for cutting out head portraits of person photographs collected by the photograph collection unit; a random ordering unit used for respectively and randomly mixing the head portrait images cut out by the head portrait cut-out unit and the head portrait cut-out photographs; a synthesis unit used for randomly combining the head portrait images with the e head portrait cut-out photographs and generating new photographs; and a storage unit used for storing the new photographs generated by the synthesis unit. According to the invention, the recombination of person photograph materials is realized through the simple terminal equipment, and more person photograph materials are formed.

The invention belongs to the field of chemical synthesis, relates to a method for preparation of glycopyrronium bromide, and especially relates to enriched high-purity (3R, 2'S,) and (3S, 2'R,) glycopyrronium bromide and a preparation method of a novel intermediate involved in the synthesis method of glycopyrronium bromide. The method provided by the invention overcomes the defect that the prior art has a low yield and can produce large pollution, can realize preparation of glycopyrronium bromide shown in the formula I, has a high yield, produces low environmental pollution and is convenient for purification. Glycopyrronium bromide obtained by the method has a melting point of 195 to 198 DEG C.

The invention discloses a method for preparing exenatide. The exenatide is prepared from a full protection fragment of Phe-Ile-Glu-Trp-Leu-Lys-Asn-Gly-Gly-Pro-Ser-Ser-Gly-Ala-Pro-Pro-Pro-Ser-CONH2 and full protection fragments of following three fragments of Met-Glu-Glu-Glu-Ala-Val-Arg-Leu-COOH, Thr-Ser-Asp-Leu-Ser-Lys-Gln-COOH and His-Gly-Glu-Gly-Thr-Phe-COOH. By means of the method, the problems that existing solid-phase-synthesis exenatide is difficult to purify and large-scale production is difficult are solved, the synthesis efficiency is improved, impurity accumulation is reduced, and the purifying difficulty is lowered.

The invention discloses a preparation method of a glucosyl modified quantum dot fluorescent probe. The preparation method comprises: adopting D-glucose as a raw material, carrying out hydroxyl complete protection and terminal glycosylation, adding a N,N-dimethylformamide solution and potassium thioacetate to catalyze, removing the protection group through sodium methoxide / methanol to obtain mercapto derivatized glucose, and modifying the mercapto derivatized glucose on the surface of quantum dots through ligand exchange to obtain the glucosyl modified quantum dot fluorescent probe. According to the present invention, the prepared glucosyl modified quantum dot fluorescent probe is used for detecting the pesticide fenpropathrin content; and the glucosyl modified quantum dot fluorescent probe has the specific recognition ability of sugar and the special properties of quantum dots, and further has advantages of good water solubility and long stabilization time, and the preparation method has advantages of short synthesis route of the glucosyl modified body, simple synthesis operation, simple preparation method of the modified quantum dots, and rapid preparation.

The invention discloses a method for preparation of a compound shown in formula (II). The method mainly includes two steps: an amination reaction and introduction of an amino protection group. The invention also discloses a method for preparation of brinzolamide through the compound in formula (II), and the method mainly consists of: sulfamation of the compound in formula (II) and amino protection group removal of the sulfamation product. According to the method, a protection group is first introduced at site C-3, then a sulfonamide group is introduced at site C-6, and finally the protection group at site C-3 is removed, so that the synthesis operations of brinzolamide become easier, the security risk and the cost are lower, and the total yield of brinzolamide is significantly enhanced. Therefore, the feasibility of large-scale industrial production and the competitive advantage of the product in the market are improved.

The invention in particular relates to a double-layer walled microporous self-assembled material with a fluorescent recognition effect and a preparation method thereof, which belong to the technical field of advanced porous materials. According to the invention, by using rigid dicarboxylic acid or rigid azacyclo organic ligands as a supporting wall of a microporous material and using a metal ion with a multi-ligand-field geometry configuration as a central metal, the microporous self-assembled material with a double-layer organic wall is prepared through a solvent hot self-assembled growth method. A porous channel of the prepared microporous self-assembled material with the double-layer organic wall has a size of 5-20 angstroms and is a three-dimensional interconnected porous channel. The microporous self-assembled material provided by the invention has the advantage of characteristic fluorescence; and the fluorescence is weakened and obviously red-shifted when the microporous self-assembled material meets nitrobenzene explosive compounds, so that a recognition purpose is achieved. The double-layer walled microporous self-assembled material with the fluorescent recognition effect, provided by the invention, has the advantages of simple synthesis method and strong controllability and has broad application prospects in inspection and detection aspects of the nitrobenzene explosive compounds.

The invention relates to a preparation method of canagliflozin hemihydrate and monocrystal thereof, belonging to the technical field of canagliflozin hemihydrate. The method comprises the following steps: crystallizing the raw material 5-iodo-2-methyl benzoic acid by using canagliflozin hemihydrate monocrystal as a crystal seed to prepare the canagliflozin hemihydrate, and carrying out solvent volatilization in a methanol-water solvent environment to prepare the canagliflozin hemihydrate monocrystal. The preparation method of the canagliflozin hemihydrate is simple, has the advantages of high yield and low cost, and is suitable for industrial production. The preparation method of the canagliflozin hemihydrate monocrystal is simple and convenient, and can obtain the high-quality monocrystal compound.

The invention relates to a preparation method of a metallic organic macrocyclic crystalline-state material for splitting chiral amine. The method firstly comprises the following steps: firstly synthesizing a chiral ligand (1R,2R)-H2L, wherein the chiral ligand (1R,2R)-H2L is (1R,2R)-N-2-hydroxyl-3-tertbutyl-5-(4-pyridine)benzylene-N'-2-hydroxyl-3-tertbutyl-5-(4-pyridine)benzyl-cyclohexanediamine; then preparing the metallic organic macrocyclic crystalline-state material for splitting chiral amine by adopting a solvothermal method. Compared with the prior art, by adopting the solvothermal method, the preparation method is low in reaction temperature, short in reaction time, low-cost in reaction raw materials, and easy to prepare, as well as simple for synthesis operations, without the need of complicated aftertreatment, the prepared chiral metallic organic macrocyclic crystalline-state material is very stable in structure, strong in selective adsorption capability, and high in splitting efficiency.

The invention discloses a synthesis method of a cyclic dipeptide. A cyclic dipeptide sequence contains L-asparagine or L-glutamine. The method comprises the following steps: by taking 2-Chlorotrityl Chloride Resin as a carrier, carrying out solid-phase synthesis to obtain a straight-chain dipeptide fragment H-Glu-AA-OH or H-Asp-AAOH, wherein AA is other alpha-amino acids except asparagine, glutamine, glutamic acid, aspartic acid and cysteine; then carrying out a methyl esterification reaction to obtain straight-chain dimethyl ester protected dipeptide H-Glu (OMe) -AA-OMe or H-Asp (OMe)- AA-OMe; then carrying out water-phase alkaline cyclization to obtain cyclic dipeptide Cyclo[ Glu (OMe)- AA] or Cyclo[ Asp (OMe)- AA] protected by side chain carboxyl methyl ester; and finally, carrying outammonolysis to obtain the cyclic dipeptide containing glutamine or asparagine. The method is simple in synthesis process and safe to operate, incomplete cyclization caused by steric hindrance of aminoacid side chain protecting groups in the cyclization process is effectively avoided, few byproducts are produced, purification is easy, and cyclic dipeptide containing Gln and Asn can be synthesizedin batches.

The invention relates to a method for synthesizing a titanium silicalite molecular sieve, which comprises the following steps: mixing, stirring and hydrolyzing a titanium-containing compound, a TPAOH aqueous solution and a silicon raw material, and putting the obtained mixture into a high-pressure reaction kettle to heat for reacting; and mixing an obtained reaction mixture with solid silica gel, drying the obtained object so as to obtain a solid mixture, carrying out heating reaction on the solid mixture in an airtight reaction kettle, after the solid mixture is cooled, taking out and then roasting the solid mixture so as to remove organic matters, so that a TS-1 molecular sieve is obtained. In the technical scheme above, by reducing the application amount of a guiding agent tetrapropylammonium hydroxide (TPAOH), taking inorganic silicon oxide for replacing organosilicone as a raw material, and taking a solid-phase solvent-free crystallization method, the steps of filtering, washing and the like are omitted, thereby simplifying the synthesis operation of the TS-1 molecular sieve and reducing the synthetic cost.

The invention discloses a non-noble metal diatomic electrocatalyst, and a preparation method and an application thereof. The catalyst contains, by mass, 1-7 parts of W, 1-7 parts of Mo, 79-81 parts ofC, 4-6 parts of N and 6-8 parts of O. Sodium tungstate and ammonium molybdate which are used as metal precursors and graphene rich in oxygen-containing functional groups undergo hydrothermal self-assembling, then the obtained material is freeze-dried, and a chemical vapor deposition process is carried out in an ammonia / argon atmosphere to prepare the W / Mo diatomic electrocatalyst, which interactswith nitrogen-doped graphene by oxygen atom anchoring. The non-noble metal diatomic electrocatalyst obtained in the invention has an electrocatalytic hydrogen evolution performance, and has the advantages of high activity, low initial potential, large current density, small Tafel slope, stable performances and the like.

The invention relates to a synthesis method of imatinib and imatinib mesylate. The method comprises the following steps: condensing 3-acetylpyridine and N,N-dimethylformamide dimethyl acetal which aretaken as initial raw materials to obtain 3-dimethylamino-1-(3-pyridyl)-2-propen-1-one, then reacting with 2-methyl-5-nitrophenylguanidine nitrate to form a pyrimidine ring, performing nitro reductionto obtain N-(5-amino-2-methylphenyl)-4-(3-pyridyl)-2-pyrimidinamine, amidating the N-(5-amino-2-methylphenyl)-4-(3-pyridyl)-2-pyrimidinamine and 4-(chloromethyl)benzoyl chloride, performing affinitysubstitution with 1-methylpiperazine to obtain imatinib, and salifying the imatinib and methanesulfonic acid. The products obtained by the method have the advantages of few impurities, simplicity in post-treatment, high total yield, greenness, environmental protection and safety, and is suitable for a production process for large-scale industrial production of imatinib mesylate.

The invention relates to a method for preparing a phosphorescence manganese compound. The method includes carrying out reaction on 3, 6-di-iodine-N-tosyl carbazole, 3-6-di-tert-butyl carbazole, copperpowder and K2CO3 to obtain 3, 6-bis-(3, 6- di-tert-butyl carbazole N-) carbazole-N-tosyl carbazole; carrying out reaction on the 3, 6-bis-(3, 6- di-tert-butyl carbazole N-) carbazole-N-tosyl carbazole and KOH to obtain compounds TCz; carrying out reaction on the compounds TCz, t-BuOK and dibromo alkane to obtain compounds TCz-R'; carrying out reaction on the compounds TCz-R' and PPh3 to obtain compounds L; carrying out reaction on the compounds L and MnBr2.4H2O to obtain the phosphorescence manganese compound. The method has the advantages that synthesis operation is simple, the method is lowin cost, products are high in luminescence quantum efficiency and current carrier efficiency, and luminescence materials and transporting materials which are good in performance can be obtained by the aid of the method.

The invention relates to a molecular sieve preparation method, and aims at providing a method for synthesizing all-silicon ZSM-51 zeolite by a seed crystal guiding method. The method comprises the following steps: taking a silicon source, an alkali source and ethanol, mixing with all-silicon ZSM-51 zeolite seed crystal, and then placing in a mortar to grind; afterwards, transferring into a reaction kettle, and performing crystallization reaction for 12h-3d at 160-200 DEG C; enabling products to be subjected to suction filtration and dried to obtain the all-silicon ZSM-51 zeolite. According tothe method, by using nontoxic harmless ethanol as a pore passage filling agent, the seed crystal is used for guiding, and toxic organic matter is prevented from use; and synthetic operation is simpleand easy. The yield of the products can be greatly improved, and the synthetic operation is simple and easy. The prepared products keep good crystallinity and purity, and have good reaction activity.No water is added in a whole synthetic system, a solid phase state is kept all the time in the synthetic process, and unnecessary exhaust gas and waste liquor discharge and loss are reduced in the production process. The adopted inorganic raw materials are all friendly to the environment and relatively low in price, thereby having important significance in the actual chemical production field.

The invention discloses a synthesis method of 2-(difluoromethyl)pyridine-3-ol, and belongs to the field of organic chemical synthesis. The method comprises the following steps: dissolving 3-methoxypyridine-2-formaldehyde into an organic solvent, and performing reaction with diethylamino sulfur trifluoride under the protection of nitrogen to obtain 2-(difluoromethyl)-3-methoxypyridine; and reactingthe 2-(difluoromethyl)-3-methoxypyridine with an acid to obtain the target product 2-(difluoromethyl)pyridine-3-ol. The method is reasonable in process design, short in route, simple in synthesis operation and easy to implement.

The invention discloses an 8-cyclohexyl-2-fluoro-vidarabine, a preparation method thereof and an application of 8-cyclohexyl-2-fluoro-vidarabine to treatment of leucocythemia. By using a synthesis method disclosed by the invention, a heavy metal catalyst in the current synthesis method is avoided, the synthesis operation is simplified, heavy metal residues in 8-cyclohexyl-2-fluoro-vidarabine are avoided, and the preparation method is suitable for research and further large-scale preparation of drugs.