117 results about "Sodium cyanoborohydride" patented technology

The invention relates to a new protein quantitative method, in particular to a quantitative method utilizing equiponderance dimethylation marking. The method utilizes the organic combination of methanal and isotope of the methanal, and sodium cyanoborohydride and isotope of the sodium cyanoborohydride for marking peptide fragments, so that the peptide fragments have the similar mass-to-charge ratio on the primary spectrum of the mass spectrum and have the different mass-to-charge ratios on the secondary spectrum of the mass spectrum, and the protein quantitative analysis is achieved on the secondary spectrum. Compared with other quantitative methods, the method has the advantages of being high in quantitative accuracy and precision, and wide in dynamic range.

The present invention relates to a clopidogrel hydrogen sulfate preparation method. According to the clopidogrel hydrogen sulfate preparation method, 2-thiophene aldehyde is adopted as a basic starting material, the 2-thiophene aldehyde and o-chlorophenylglycine methyl ester are subjected to a condensation reaction to produce the corresponding imine intermediate, the imine intermediate is reduced into the corresponding secondary amine intermediate by adopting sodium borohydride or by directly adopting sodium cyanoborohydride intermediate, the secondary amine intermediate and formaldehyde are subjected to reaction ring closure to obtain clopidogrel, and the clopidogrel is acidified with sulfuric acid to obtain the target compound clopidogrel hydrogen sulfate. According to the present invention, the provided synthesis route is short, the related reactions are classical organic reactions, the reaction conditions are mild, the operation is simple, the total yield is high, the cost is low, and the preparation method is suitable for industrial production.

The invention discloses a method for treating industrial waste water containing heavy metal contaminants by utilizing industrial fly ash and nano iron. The method comprises the following steps of: firstly, fully mixing industrial fly ash and a ferric chloride solution at room temperature; and secondly, dropwise adding sodium cyanoborohydride to the mixed solution to reduce trivalent iron ions to zero-valent nano iron, and loading onto fly ash particles to obtain a fly ash-nano iron composite material. The fly ash-nano iron composite material is added to the industrial wastewater containing heavy metal contaminants, and is treated and recovered at normal temperature. The precipitated supernatant can meet the relevant integrated wastewater discharge standards to be directly discharged, wherein the zero-valent nano iron accounts for 10% of the composite material in mass, the concentration of the wastewater containing heavy metal contaminants is less than or equal to 100 mg / L, and the pH value of the wastewater containing heavy metal is 5.6 to 9. The method has the advantages of making full use of nano-sized silica particles with a large specific surface area in fly ash, improving the removal rate of the industrial wastewater containing heavy metal contaminants, solving the problems that the nano iron is easily oxidized and agglomerated, and adsorbents are difficultly recovered and the like, improving efficiency and saving cost, and achieving the purpose of water environmental pollution reduction and recovery and comprehensive utilization of resources.

The invention provides a glucan-adriamycin conjugate drug, which adopts the structure shown in the formula (I) or the formula (II) of the Specification, and n is the degree of polymerization of the glucan and is equal to or greater than 10 and equal to or smaller than 3125. According to the invention, the glucan, sodium cyanoborohydride and adriamycin are used as raw materials to prepare the glucan-adriamycin conjugate drug; as the glucan as a raw material has good biological activity and biocompatibility, the prepared glucan-adriamycin has good biological activity and biocompatibility; besides, the glucan is connected with the adriamycin through an oxime bond, so that the glucan-adriamycin conjugate drug can be released quickly in tumor tissue or a cell under the condition of relatively low pH value, so that the drug effect is improved; reduced glucan-adriamycin conjugate drug adopting the structure of the formula (II) of the Specification has relatively stable performance, and the adriamycin can be released relatively slowly, so that ideal long-acting therapy can be realized.

The invention discloses chitosan derivative hydrogel and a preparation method and application thereof. A chitosan derivative has a structural formula (please see the formula in the description); in the formula, m is any natural number from 930 to 1550, n is any natural number from 2 to 19, and R is C8-C18 straight-chain hydrocarbon. The preparation method of the hydrogel includes the following steps of firstly, dissolving fatty alcohol polyether in solvent, adding dimethylsulfoxide, adding pyridine and trifluoroacetic acid, and conducting a sufficient reaction; secondly, adding dicyclohexylcarbodiimide to obtain fatty alcohol polyether with glyoxyl at the tail end; thirdly, dissolving the product in the second step and chitosan in mixed solvent, and adding sodium cyanoborohydride to obtain the chitosan derivative with a fatty alcohol polyether structure on a side chain; fourthly, adding water to the chitosan derivative in the third step to obtain the hydrogel. The hydrogel has temperature sensitivity, is in a sol state at a low temperature and in a gel state at a high temperature, can be used as injectable type hydrogel, and can be used for preparing a medical filling material and a medical releasing system.

The invention relates to a quaternization N-ethyl chitosan, which is a novel chitosan ramification with a good water-solubility, bacteriostasis, moisture absorption, moist storage and emulsification stability. The preparation process is characterized in that: under the pH of 3.0 to 12.0, the chitosan of the deacetylation of 30 percent to 90 percent is reacted with pyruvic acid and malonaldehydic acid to generate a chitosan Schiff base, and is deoxidized by sodium borohydride, potassium borohydride, sodium borohydride cyanoacrylate, cyano-group sodium borohydride and the mixture to obtain the N-ethyl chitosan; the N-ethyl chitosan in alcohol medium is processed by alkali, and is modified by glycidyl trimethyl ammonium chloride or 3-chlorine -2-hydroxy trimethyl ammonium chloride so as to get N-ethyl chitosan admixture with quaternization; the admixture is washed and dissolved by methyl alcohol or ethanol solution, then dialysis desalination, concentration in decompression or atmospheric pressure, absolute ethyl alcohol, or acet sedimentation and dehydration are conducted, finally the admixture is arranged in a vacuum airer at 60 DEG C to 150 DEG C for drying for vacuum freeze drying until the water volume is less than 10 percent.

The invention provides a preparation method of a novel natural active polypeptide Tubulysin U. The preparation method comprises the following steps: dissolving a compound 2 in trifluoroacetic acid, heating under reflux to prepare an intermediate, reacting with a compound 3 and diisopropylethylamine to obtain a product, reacting the product with 2, 6-dimethylpyridine and tert-butyldimethylsilyltrifluoromethanesulfonate, adding sodium hydroxide after the reaction to prepare an intermediate acid, reacting the intermediate acid with a compound 6, HATU and diisopropylethylamine to obtain a product,adding triphenylphosphine to prepare an intermediate amine, adding a compound 8 and HATU to react, adding ammonium fluoride to prepare a first intermediate, adding sodium hydroxide to the first intermediate to prepare a second intermediate, adding acetic anhydride to the second intermediate to prepare a third intermediate, adding trifluoroacetic acid to the third intermediate to prepare a fourthintermediate, and adding formaldehyde and sodium cyanoborohydride to the fourth intermediate to react, thereby obtaining the target product. The structures of the compound 2, compound 3, compound 6 and compound 8 are disclosed in the specification.

The invention provides an isotope derivatization reagent for labeling amino/phenolic hydroxyl and a synthesis method thereof and belongs to the field of chemical synthesis. A homologous compound of p-aminophenylacetic acid containing amino, a benzene ring and carboxyl in a structure or a homologous compound of 4-(2-aminoethyl)benzoic acid is used as a raw material; and the amino is dimethylated and then the carboxyl in the product is subjected to esterification by adopting N-hydroxysuccinimide to obtain the isotope derivatization reagent. The isotope derivatization reagent has structure characteristics that one part of the isotope derivatization reagent is succinimidyl ester and the other part of the isotope derivatization reagent is dimethyl substituted tertiary amino; the succinimidyl ester is connected to dimethylamino through a carbon chain and a benzene ring; and the number of carbon atoms on the benzene ring and the carbon chain which is connected to the amino is 0 to 6. According to the isotope derivatization reagent provided by the invention, different D substituted or <13>C substituted formaldehyde, or H or D substituted sodium cyanoborohydride are selected and a reactionroute is adjusted to obtain a series of isotope labeled reagents which can efficiently react with amino or phenolic hydroxyl and have different isotope substitutions. A starting raw material is changed, and the isotope labeled reagents with similar functions can be prepared through the method.

The invention relates to the field of preservation of cultural relics technology, and discloses a preparation method for silk fiber used for protecting textile cultural relic. The preparation method comprises: 1), adding cyclodextrin and o-iodoxy potassium benzoate into dimethyl sulfoxide to react; filtering the product, adding acetone into the filtrate, filtering, dissolving the solid in water, freeze drying the filtrate after filtering to prepare cyclodextrin mono-aldehyde; 2), dipping the silk fiber in water, degumming; 3), adding the silk fiber and cyclodextrin mono-aldehyde into dilute hydrochloric acid aqueous solution, heating to react; adding sodium cyanoborohydride, reacting, removing the silk fiber to wash; 4), putting the silk fiber into an impregnation liquid, removing and drying to prepare the final finished product. The prepared silk fiber can purify air, has antibacterial and antiscolic effects, and can be made into bottom liner of the cultural relic, inner packing of the cultural relic, and set lining cloth of cultural relic display case. The textile cultural relic can be protected in close distance, and the damage suffered by the cultural relic can be avoided effectively.

The invention relates to a preparation method and application of a fluorescent copper cluster with stable silane. According to the method, a silane coupling agent frequently used in the industry is adopted, 2-mercaptopropyl trimethoxy silane is used as a stabilizer, and through the high substantivity of a mercapto functional group of the 2-mercaptopropyl trimethoxy silane with copper, and the moderate reducing capacity of sodium cyanoborohydride, copper salt is reduced to generate a silane blocking fluorescent copper cluster. The method has the characteristics of being easy to implement, free of shielding of extra surface active agents or inert gas, and low in cost. The copper cluster obtained through the method is composed of 4-9 copper atoms, and can emit two-peak fluorescent light with the peaks at wavelength positions of 410 nm and 580 nm when triggered by ultraviolet light with the wavelength being 375 nm. Through research, the fluorescent copper cluster can be applied to low concentration hydrogen peroxide detection and has certain practical application value.

The invention discloses a group-A neisseria meningitides capsular polysaccharide conjugated vaccine and a preparation method. The preparation method comprises the following steps of: dissolving purified group-A neisseria meningitides capsular polysaccharide in water, heating, and adding hydrogen peroxide to react; performing ultrafiltration and removing impurities, and concentrating to obtain depolymerized meningococcal liquid; adding ADH (antidiuretic hormone) and EDAC (carbodiimide) to react, adding sodium cyanoborohydride to react, and performing ultrafiltration and removing impurities to obtain derived group-A meningococcal capsular polysaccharides; dissolving the derived group-A meningococcal capsular polysaccharides and vector protein CRM197 in buffer liquid, regulating pH, and adding 1-(3-dimethylaminopropyl)-3-ethylcarbodimide hydrochloride to react. The vaccine with molecular weight of over 200KD has stronger immunogenicity. The method is simple in process flow, high in yield and low in production cost, and the polysaccharide-protein ratio is relatively stable and can be controlled by human being, so that the quality stability of combined products can be greatly improved.

The invention provides an alginic acid-adriamycin amycin bonding medicine which has a structure shown in a formula (I) or (II), wherein n is degree of polymerization of alginic acid, and n is greater than or equal to 7 but less than or equal to 1507. The alginic acid-adriamycin amycin bonding medicine is prepared by taking alginic acid, sodium cyanoborohydride and adriamycin amycin as raw materials. As the raw material alginic acid ahs good bioactivity and biocompatibility, the alginic acid-adriamycin amycin prepared has good bioactivity and biocompatibility. Meanwhile, alginic acid and adriamycin amycin are connected through oxime bonds, and can be quickly released in a tumor tissue or cell under a lower pH value condition, so that the pesticide effect is enhanced. The reductive alginic acid-adriamycin amycin bonding medicine with the structure shown in the formula (II) further has a more stable performance, is more slowly to release adriamycin amycin, and reaches an ideal long-acting treatment.

The invention provides a method for preparing N-benzylhydroxylamine and hydrochloride thereof. The method is characterized in that oximation reaction is first carried out, which is to use water to dissolve hydroxylamine hydrochloride, add 25 percent NaOH solution, lower temperature to about 20 DEG C by use of ice water, drip benzaldehyde at a temperature between 20 and 30 DEG C and then stir for reaction at a room temperature; reactant is kept to stand for 30 minutes so as to be layered; oily matter in a lower layer is separated out and rinsed once, dried by use of anhydrous MgSO4 and filtered so as to obtain brown oily matter, namely benzaldehyde; the benzaldehyde is reduced by use of sodium cyanotrihydroborate, extracted and purified so as to obtain the N-benzylhydroxylamine; and finally the N-benzylhydroxylamine is salified by leading in hydrogen chloride so as to obtain the N-benzylhydroxylamine hydrochloride. The method has the advantages that raw materials for reaction are low in price and easy to get, and the method is mild in reaction, simple and stable in conditions and easy to expand production.

The invention relates to a preparation method of a sitafloxacin hydrate five-membered ring side chain intermediate. The preparation method comprises following steps: keto carbonyl groups of a raw material 1 are reacted with sodium cyanoborohydride or sodium triacetoxyborohydride in the presence of ammonium acetate or ammonium chloride; reduction of amide carbonyl groups of an obtained production is realized with lithium aluminum hydride; free amino groups of a reduction product are reacted with di-tert-butyl dicarbonate ester in the presence of an alkali; phenethyl groups of an obtained compound are subjected to reductive destruction with formic acid or a formate in the presence of palladium-carbon so as to obtain the sitafloxacin hydrate intermediate (product 5). Reaction conditions of the preparation method are mild; equipment requirements are low; preparation process is safe; stereoselectivity is excellent; the raw material reagents are cheap and easily available; and production cost is low.

The invention relates to a magnetic dendritic polymer composite magnetic nanoparticle, and a preparation method and application thereof, and belongs to the technical field of chemical material preparation. According to the preparation method, an amino modified ferriferrous oxide nanoparticle is added into glutaraldehyde and anhydrous methanol, and the mixture is mechanically stirred for a period of time and filtered with suction; the obtained product is washed with anhydrous methanol and centrifuged; the obtained precipitate is transferred to a one-neck flask containing anhydrous methanol, andfour-arm polyethylene glycol amine is added to the formed black suspension; mechanical stirring is performed under a water bath condition, and sodium cyanoborohydride with an equal amount is added during the stirring by stages; and after the stirring is finished, the product is separated out by a magnet, is washed with anhydrous ethanol and deionized water, and is centrifuged, placed in a vacuumoven and dried under vacuum. The prepared magnetic dendritic polymer composite nanoparticle is used for immobilization of cellulase. The magnetic dendritic polymer composite material synthesized by the preparation method has the superparamagnetic property, and the immobilization of cellulase can improve the enzymatic activity and the storage stability of the cellulase, thereby achieving reuse of the cellulase.

The invention belongs to the field of chemical synthesis. The invention relates to a method of synthesis of 6-deoxy-L-talose,including: 1) performing glucoside protection of 1-positon hydroxyl of L-rhamnose in methanol solution by utilizing cation exchange resin (732H+type) to obtain a compound; 2) performing isopropylidene protection of hydroxyls at 2 and 3 positions of the compound to obtain a compound; 3) oxidizing 4-position hydroxyl of the compound to a ketone carbonyl group by utilizing a Swern oxidation system, so as to obtain a compound; 4) performing stereoselective reduction of 4-position carbonyl of the compound by utilizing sodium borohydride or sodium cyanoborohydride, so as to obtain a precursor compound with an opposite configuration to the raw materials, of 6-deoxy-L-talose; 5) refluxing the compound in sulfuric acid aqueous solution to hydrolyze to obtain 6-deoxy-L-talose. The preparing method using easily-available L-rhamnose having low price as the initial raw material, is a simple method, and is utility and efficient.

The invention provides a preparation method of a municipal sewage treating agent.The method comprises the steps of firstly, picking dry straw, pulverizing the straw, adding a solution of sodium cyanoborohydride, ammonium ceric nitrate and gelatin, mixing the materials to be uniform, raising the temperature, then adding poly(ethyl acrylate), polyacrylonitrile and glutaraldehyde, raising the temperature, lowering the temperature, and conducting filtering, so that solid matter is obtained; then adding etidronic acid and polyhydric alcohol phosphate ester to water, conducting stirring, adding isothiazolinone, sepiolite, starch xanthate, magnesium sulfate heptahydrate, chitosan, N, N-dimethyl methylene diphosphonic acid, lecithin and lignin, and mixing the materials to be uniform, so that a mixture (I) is obtained; finally, adding a sodium hydroxide solution to the mixture (I) to adjust pH to 6.0-7.0, adding organic acid and the obtained solid matter, mixing the materials to be uniform, and then leaving the mixture standing still, so that the municipal sewage treating agent is obtained.By means of the municipal sewage treating agent, the chemical oxygen demand of sewage can be lowered to 63 mg/L, the biochemical oxygen demand can be lowered to 28 mg/L, suspended solids can be decreased to 35 mg/L, and total phosphorus can be decreased to 0.37 mg/L.

The invention provides a synthesis method for a key intermediate, analogue or salt of ticlopidine. The synthesis method comprises the following steps of: (1) adding 6-nitro-2,3-dichlorobenzaldehyde and glycine or corresponding substituted glycine into a solution and adding a reducing agent to completely react to obtain N-(6-nitro-2,3-dichlorobenzyl) glycine and an analogue thereof; and (2) completely reacting the N-(6-nitro-2,3-dichlorobenzyl) glycine and the analogue thereof under the action of a catalyst to obtain the key intermediate, analogue or salt of the ticlopidine, wherein the solution in the step (1) is a mixed solution of a protic solvent and an inorganic base, and the reducing agent is one or a mixture of sodium borohydride, potassium borohydride, lithium borohydride, sodium cyanoborohydride and acetic sodium borohydride. The method is simple in operation, mild and easily-controlled in condition, convenient for aftertreatment, environment-friendly and higher in yield, and is a brand new efficient industrial synthesis method for the key intermediate, analogue or salt of the ticlopidine.

The invention discloses a method for detecting a residual quantity of sodium cyanoborohydride in a protein sample or product. The method comprises the steps of subjecting the protein sample or product to pretreatment including protein removal, then, adding the pretreated protein sample or product into a mixed solution of a Coomassie brilliant blue G-250 solution and a polysorbate 20 solution so as to form a mixture system, determining the light absorbancy of the mixture system by adopting an ultraviolet-visible spectrophotometer, and finally, determining the content of sodium cyanoborohydride in the protein sample or product by using an external standard method, wherein an external standard substance of the external standard method is sodium cyanoborohydride. The method has the advantages of simple operating steps, quickness, low cost and low toxicity.

The invention relates to the field of biological pharmacy, and provides a new medicine compound for treating tumors, and particularly relates to an autophagy inhibitor and arginase medicine compound and application thereof. The medicine compound is used for treating the tumors. According to the medicine compound, the antineoplastic activity of arginase can be obviously strengthened in vitro; the immunogenicity of a person for recombing the arginase can be reduced; and the half-life period of the arginase in vivo can be prolonged. The arginase modified by poly-sialic acid is provided; and the arginase modified by the poly-sialic acid is characterized in that the active activated poly-sialic acid is reacted with the arginase under the condition that sodium cyanoborohydride exists to form conjugates. By means of the autophagy inhibitor and arginase medicine compound, the killing effect of the arginase on the tumors can be strengthened, the curative effect of the arginase can be strengthened, and the curative effects of the arginase on treating the melanin tumor and the breast cancer can be strengthened.

The invention provides a lentinan-adriamycin bonding medicine which has the structure shown in the formula (I) or formula (II) in the Specification, wherein n refers to the polymerization degree of lentinan, and is not less than 10 and not greater than 3278. According to the invention, lentinan and adriamycin are used as raw materials, or lentinan, sodium cyanoborohydride and adriamycin are used as raw materials to prepare two types of lentinan-adriamycin bonding medicines; as the lentinan used as the raw material has excellent biological activity and biocompatibility, and small toxic and side effects, the prepared lentinan-adriamycin bonding medicines have excellent biological activity and biocompatibility, and lower toxic and side effects; in addition, the lentinan and adriamycin are connected through oxime bonds, and can be quickly released in the tumor tissue or cells with the lower pH value, so that the efficacy of the lentinan-adriamycin bonding medicine is improved; the reduced lentinan-adriamycin bonding medicine which has the structure shown in the formula (II) in the Specification is more stable in performance, and the adriamycin can be released more slowly, so that the ideal long-acting treatment is realized.