55 results about "Glucal" patented technology

The invention discloses a method for on-line synthesizing glucose-6-acetate catalyzed by lipase. According to the method, glucose and vinyl acetate with a molar ratio being 1 : 16-22 are used as raw materials; 0.5-1.0 g of the lipase (Lipozyme TLIM) is used as a catalyst and a mixed solvent formed by tert-amyl alcohol and DMSO is used as a reaction solvent. The lipase (Lipozyme TLIM) is uniformly filled in a reaction channel of a microfluidic channel reactor, wherein the inner diameter of the reaction channel of the microfluidic channel reactor is 0.8-2.4 mm, and the length of the reaction channel is 0.5-1.0 m; the raw materials and the reaction solvent are continuously introduced into the reaction channel for an acylation reaction, wherein the temperature of the acylation reaction is controlled at 40-55 DEG C and the time of the acylation reaction is 15-35 min; a reaction liquid is collected on-line; and the glucose-6-acetate is obtained after the reaction liquid is subjected to conventional post-treatment. The method provided by the invention has the advantages of short reaction time, high selectivity and high yield.

A method for preparing 5-acetoxymethyl furfural with carbohydrate at normal pressure comprises the following steps: adopting fructose or glucose as raw material and dimethylsulphoxide as reaction medium to produce 5-methylol furfural through dehydration in the present of solid acid catalyst, cooling the obtained products, removing the solid acid, removing the water generated in the dehydration reaction with 4A molecular sieve, separating the molecular sieve through filtration and then adding anion-exchange resin of which anions are displaced by acetate and acetic anhydride to perform acetylation reaction to generate 5-acetoxymethyl furfural. The method has high yield, mild reaction conditions, cheap and accessible raw materials and catalyst, the catalyst can be recycled and the whole process is non-corrosive to devices and environmentally friendly.

The invention relates to a coumarin compound acidulated by glucal and application thereof. The compound has a structure showed in the right formular, wherein R is one of-H, -OH, -CH3, -OCH3, -NH2 or ester group; and R1, R2, R3 and R4 are one of -H, -OH, -CH3, -SH, -OCH3, -NH2 or glucal acid group. The coumarin compound acidulated by the glucal has the activities of resisting arthritic and tumor.

The invention discloses a method for preparing 4, 6-dibenzyl-2, 3-unsaturated glucoside, which is characterized by comprising the following steps of: mixing 3, 4, 6-tri-O-benzyl glucal and dichloromethane, acetonitrile, tetrahydrofuran, N, N-dimethylformamide, acetone or diethyl ether in a molar volume ratio of 1 mol: (5-50) L, adding a sulfuric acid / silica catalyst and an oxygen- or sulfur-containing nucleophilic receptor under stirring, undergoing a rearrangement reaction of 3, 4, 6-tri-O-benzyl glucal at a temperature of 0-50 DEG C, filtering out the catalyst after the reaction ends, and concentrating the filter liquor to obtain the 4, 6-dibenzyl-2, 3-unsaturated glucoside. The method for preparing the 4, 6-dibenzyl-2, 3-unsaturated glucoside has the advantages of simple process, convenience in operating, high yield, low production cost and no environmental pollution; the reagent used for synthesis is cheap and easy to get; the dissolvent is cheap and easy to get and has little toxicity; and the method for preparing the 4, 6-dibenzyl-2, 3-unsaturated glucoside is a method for an Ferrier rearrangement reaction of 3, 4, 6-tri-O-benzyl glucose ene with a very good application prospect.

The invention discloses a method for preparing 4,6-dibenzyl 2,3-unsaturated glucoside. The method is characterized by comprising the following steps of: mixing 3,4,6-tri-O-benzyl glucal and dichloromethane in a mole / volume ratio of 1mmol: (10-40)ml, adding an acceptor with stirring, performing 3,4,6-tri-O-benzyl glucal rearrangement reaction at room temperature under the action of a FeCl3 / C solid acid catalyst, concentrating and purifying the filtrate after the reaction is finished, and thus obtaining the 4,6-dibenzyl 2,3-unsaturated glucoside. Compared with the prior art, the method has the advantages that: the method has simple process, low production cost, high yield and milder reaction conditions, is convenient to operate, avoids the use of high-toxicity chemical raw materials, does not pollute the environment, and is a method for synthesizing a 3,4,6-tri-O-benzyl glucal rearrangement product with the advantages of wider substrate application range, environment friendliness, economical efficiency and high efficiency.

The present invention provides a process for the synthesis of 2-deoxy-D-glucose comprising haloalkoxylation of R-D-Glucal wherein R is selected from H and 3, 4, 6-tri-O-benzyl, to obtain alkyl 2-deoxy-2-halo-R-alpha / beta-D-gluco / mannopyranoside, converting alkyl 2-deoxy-2-halo-R-alpha / beta-D-gluco / mannopyranoside by reduction to alkyl 2-deoxy-alpha / beta-D-glucopyranoside, hydrolysing alkyl 2-deoxy-alpha / beta-D-glucopyranoside to 2-deoxy-D-glucose.

The invention discloses a method for producing N-acetyl-glucosamine by using insect chitinase to degrade solid chitin. According to the method, the solid chitin in a crystal state is used as a substrate to perform hydrolysis, and a composite enzyme used in the hydrolysis is chitinase H with a final concentration greater than 0.3mg / mL and chitinase I with a final concentration greater than 0.06mg / mL; and beta-N acetylhexosaminidase 1 with a final concentration greater than 0.06mg / mL can also be added. The method of the invention also comprises a pretreatment step of solid chitin, i.e., the solid chitin is crushed to serve as a substrate for producing the N-acetyl-glucosamine, the amount of a monosaccharide product is determined by virtue of a potassium ferricyanide method, the composite enzyme is used for degrading the solid chitin substrate, so that the conversion of more than 81 percent of substrate can be realized in 5 hours, and the industrialized application prospect is good.

The invention discloses a method for synthesizing 1,2-propylene glycol using glucose, and belongs to the fields of environment protection and energy technology. The method is the technology which is characterized in that glucose of high density is used as a raw material, CuNi / MgO is used as a catalyst, and a two-stage intermittent reaction is used for producing 1,2-propylene glycol. A glucose solution is injected into a high pressure reaction vessel, and a hydrogenolysis catalyst is added for initiating a reaction; a carrier MgO with alkalescence is used for replacing the added solid alkali, so that the reaction is carried out under a neutral condition; the two-stage intermittent reaction is carried out, thereby avoiding influence of the high temperature polymerization on the reaction, a hydrogenolysis / hydrogenation reaction of glucose is carried out at low temperature for generating an intermediate product; after heating, the intermediate product is reacted further; after cooling, filtering and separating of the product, a low carbon polyhydric alcohol whose main component is 1,2-propylene glycol is obtained. According to the invention, the concentration and the reaction selectivity of the reaction raw material are increased, and the requirement of the reaction equipment is reduced, and the operation safety coefficient of the apparatus is increased.

The invention discloses a method for synthesizing cytidine phosphinylidyne compounds through oriented catalysis. The method uses CMP, choline chloride and phosphate ions as substrate, glucose as energy donor and permeable microbial cells as enzyme source and changes the reaction temperature to prepare cytidine phosphinylidyne compounds in the reaction system through oriented catalysis. The method of the invention can be used to produce any one of three substances according to demands, the reaction system is simple and nontoxic, the production cost is low, the control method is simple and practical, and the industrial production and control are greatly facilitated. When CMP is used as substrate, the yield rate of CDP, CTP and CDP-choline are separately 80%, 91.8% and 93.3%.

The invention discloses a keto group reduction catalytic system construction and cyclic operation method. The method comprises the following technical implementation steps that a carrier is used for conducting co-immobilization treatment on reductase for catalyzing a keto group reaction and glucose dehydrogenase for catalyzing regeneration of coenzyme to prepare immobilized multi-enzyme; a keto group reduction cyclic catalysis system composed of an immobilized multienzyme reactor, a product extraction device and a 300-600Da nanofiltration device is adopted; in the immobilized multienzyme reactor, coenzyme is free in a reaction solution and cooperates with the immobilized multi-enzyme, and the keto group reduction reaction and the cyclic regeneration of the coenzyme are completed. After thereaction is completed, the immobilized enzyme is filtered and recycled, and a product is extracted from filtrate; mother liquor is extracted, calcium chloride is added to remove gluconic acid, then inorganic salt is removed by the 300-600Da nanofiltration device, and meanwhile the coenzyme is recycled, so the cyclic operation of the keto group reduction catalysis system is achieved. The method has the advantages that the cost is low, the efficiency is high, the operation is simple, the product quality is high, and few impurities are generated.

The invention relates to a method for preparing 5-hydroxymethyl furfural from phosphorylation composite oxide catalysis biomass. The method comprises the following steps: 1) dissolving or dispersing abiomass raw material into water so as to obtain a water solution or a suspension; 2) performing a reaction with sodium chloride and a catalysis and extraction solvent; 3) after the reaction is completed, performing cooling separation on a catalyst, and separating the liquid by using a separation funnel, thereby obtaining a product. According to the method, a phosphorylation composite oxide solidacid is adopted as the catalyst, the acidity of the catalyst is adjusted by adjusting the ratio of the addition amount of phosphoric acid to a Ti / Si component, the catalysis performance of glucose andbiomass in preparing HMF through dehydration preparation is optimized, the problem of separating the catalyst from a product is effectively solved, repeated use is facilitated, the production cost isreduced, and the problem of environment pollution is reduced. Meanwhile, compared with a preparation method of an ionic liquid system, the double-phase system preparation method provided by the invention has an approximate yield of the HMF.

The invention discloses a microbial fermentation method for synthesizing triterpene compounds, namely a distillers yeast recombination strain SY2 containing cucurbitane dienol synthetase SgCbQ, P450 CYP87D18 and cytochrome reductase CPR, in the metabolism route of mogrol, which takes dextrose as a substrate to synthesize three new products including 11-oxygen-cucurbitane dienol, 11-hydroxy-cucurbitane dienol and 11-oxygen-24, 25-epoxy-cucurbitane dienol. The invention further discloses a metabolism route for synthesizing mogrol through cucurbitane dienol, namely the cucurbitane dienol is catalyzed through P450 CYP87D18 and synthesized into 11-oxygen-cucurbitane dienol, 11-oxygen-cucurbitane dienol is catalyzed through enzyme and synthesized into 11-hydroxy-cucurbitane dienol and 11-oxygen-24, 25-epoxy-cucurbitane dienol, and 11-hydroxy-cucurbitane dienol and 11-oxygen-24, 25-epoxy-cucurbitane dienol can be synthesized into the mogrol through other P450 or epoxide hydrolase. The invention further discloses a novel thought for obtaining more glycosylation products by catalyzing new products through glycosyl transferase. The method has significance for determining the synthesis route of mogrol and synthesizing relevant intermediate metabolites and glycosylation products through the microbial fermentation method.

The invention discloses a method for realizing pipeline production of N-(2-ethoxyl)-Beta-D-glucopyranosylamine. The method is as follows: ethanolamine and glucose at the molar ratio of between 1:1 and 5:1 are used as a raw material which is mixed with solvent to obtain a mixed solution; the mixed solution is pumped into a pipeline reactor by a metering pump to carry out amination reaction, thereby obtaining a crude product solution containing N-(2-ethoxyl)-Beta-D-glucopyranosylamine under a pressure of between normal pressure and 2.0 MPa, at the temperature of between 40 and 80 DEG C for 10 to 30 mins. The method adopted to manufacture N-(2-ethoxyl)-Beta-D-glucopyranosylamine can obtain high rate of conversion at less energy consumption.

The invention discloses a method for synthesizing choline phosphate through whole-cell biocatalysis, which comprises the following steps of: using choline chloride and phosphate ions as substrates and glucose as an energy donor; adding a micro-molecule chemical effect substance into the substrates; and synthesizing the choline phosphate by using microorganism whole-cell biocatalysis having permeability. The method for synthesizing the choline phosphate by adopting the whole-cell biocatalysis overcomes the defects that a chemical synthesis method has high cost, low conversion rate, high toxicity of a solvent and the like. In the method, the whole-cell catalysis has high stability, and the micro-molecule chemical effect substance is adopted to adjust and control the metabolic flow so as to improve the energy situ regeneration and coupling efficiencies; besides, the product concentration is greatly improved and the conversion rate is also improved.

The invention provides a method for measuring content of components of prince's-feather herb and belongs to the technical field of medicament content measurement. High performance liquid chromatography is adopted to measure the content of eight compounds, namely catechin, homo-orientin, orientin, quercetin-3-O-(2'-O-alpha-rhamnose)-betal-glucal, texifolin, luteolin-7-O-beta-D-glucoside, quercetin and kaempferide-3-0-beta-3-D-glucoside, in the prince's-feather herb under the same chromatographic condition. Compared with the conventional single component content measuring method, the method of the invention is more integral, characteristic and stable, and provides test basis for further improving the quality of the prince's-feather herb and the re-development and application of the prince's-feather herb. The invention also provides the methods for preparing reference solution and test sample solution.

The invention discloses a method for preparing 5-hydroxymethyl furfural from glucose. The method comprises the following steps: (1) adding glucose, a solid acid catalyst, a NaCl aqueous solution and ethyl acetate into a high-pressure reaction kettle, and heating to 180-200 DEG C at a stirring speed of 400-600 rpm to react, thereby obtaining a reaction phase and an extraction phase; and (2) separating the reaction phase from the extraction phase obtained in step (1), adding glucose and ethyl acetate into the reaction phase in proportion, and continuously reacting by utilizing the solid acid catalyst in the reaction phase under conditions of the step (1). The method is simple to operate, adopts cheap and easily available raw materials, adopts the green and environment-friendly catalyst, adopts ethyl acetate with a low boiling point as an extraction solvent, so that the separating and purifying of 5-hydroxymethyl furfural from glucose is facilitated, and an industrial value is realized.

The invention provides a preparation method of 2-deoxy-D-glucose, comprising the steps of adding a catalyst, an iodide and water into compound (I), allowing full reaction, extracting a reacted liquid,concentrating, and recrystallizing to obtain compound (II), wherein R1 is one of formyl, acetyl, propionyl, benzoyl, benzyl, and t-butyldimethylsilyl and the catalyst is R2CH2SCH2X; subjecting the compound (II) to deprotection, and recrystallizing to obtain 2-deoxy-D-glucose. Glucal is used herein as a start material, and catalytic hydrolysis and deprotection are performed to obtain 2-deoxy-D-glucose; the preparation process has mild reaction conditions, a reaction reagent is easy to obtain, the reaction yield is high, an intermediate purifying method is simple and easy, catalyst usage is low, catalyst removal from the product is easy, the product has high purity, the reaction time is short, and reaction yield is high.

The invention relates to a preparation method of 2-deoxy-D-glucose, which belongs to the chemical technical field. The preparation method comprises the following steps: taking 3,4,5-tri-O-acetyl D-glucal or 3,4,5-tri-hydroxy-glucal as a raw material, and is placed in a solvent under existence of solid acid, stirring and reacting for certain time under certain temperature, filtering to remove solid acid, washing the solid acid by using the solvent (the recovered solid acid enables repetitive usage), merging and filtering the solvent and then washing the solvent, adding active carbon for decolouring if necessary, filtering and removing the solvent under the pressure reduction condition after filtering the solvent, then adding a recrystallization solvent for recrystallization, cooling and filtering, washing by the recrystallization solvent, and drying under reduced pressure to obtain the white solid product 2-deoxy-D-glucose. The preparation method has the advantages of high yield, simple operation, mild condition, environmental protection, economic, and no pollution, and can be used for industrial production.

The invention provides a method for preparing 5-HMF (hydroxymethylfurfural) from glucose, and relates to 5-hydroxymethylfurfural. The method comprises the following steps that glucose, sinkaline, borax and water are mixed in a reaction container and are subjected to heating reaction; after the reaction is completed, pressure reduction distillation water removal is performed to obtain residue; hydrochloric acid is added into the residue to neutralize reaction liquid; then, choline chloride is added for fixed heating reaction; after the reaction is completed, acetonitrile is extracted obtain 5-HMF; acetonitrile is separated to obtain 5-HMF. The sinkaline and the borax are used as catalysts for catalyzing the reaction; the yield is high; the fructose is fast prepared; the fructose yield can reach 50.8 percent; the fructose can be further efficiently, fast and conveniently converted into HMF. The method has the characteristics that the method is simple; the conditions are mild; the price is low; green and environment-friendly effects are achieved, and the like. Meanwhile, isomerized catalyst choline can be sufficiently used; good economic performance is realized; the mass production can be favorably realized.

The invention relates to a method for enzymatic synthesis of feruloyl oligosaccharide in a mixed solvent. The method includes: (1) adding an activated molecular sieve in an organic solvent, and performing dehydration processing for 24-96 hours to obtain the dehydrated organic solvent; (2) performing enzymatic transesterification reaction, adding ferulic acid vinyl ester and glucose in the dehydrated organic solvent according to molar ratio of 2:1-1:6, then adding enzyme and the activated molecular sieve, performing oscillatory reaction for 10-144 hours at the temperature of 30-70 DEG C, filtering after the reaction is finished, taking clear filter liquid to perform rotary evaporation so as to remove the organic solvent, and purifying through a silicagel column. The method is simple to operate and environment-friendly, catalyst enzyme can be reused, and a structure of an obtained product is good in unicity.

[Problem]The present invention provides an industrially-preferable, cost-efficient, low-cost production method for 4-hydroxy-2-hydroxymethyl-2-cyclopenten-1-one (a compound represented by formula (I)) useful as a medicine, an agricultural chemical, or a raw material or intermediate of a medicine, an agricultural chemical, or the like.[Solution]According to the present invention, this compound represented by formula (I) is produced by subjecting an easily available compound represented by formula (II) (tri-O-acetyl-D-glucal) to a heating reaction in pressurized water.

The invention discloses an application of D-glucal in inhibiting generation of aflatoxin. The invention provides an application of D-glucal in inhibiting generation of aflatoxin. The invention also provides an application of D-glucal in preparing an inhibitor for inhibiting generation of aflatoxin. Proven by experiments of the invention, D-glucal can inhibit the generation of aflatoxin and prevent aflatoxin from harming people.

The invention relates to the technical field of organic chemistry, in particular to a preparation method of glucal. 1-acetyl glucopyranosyl bromide is added in phosphate buffer solution which contains zinc powder and copper sulfate or the zinc powder and the 1-acetyl glucopyranosyl bromide are added in sodium dihydrogen phosphate water solution, stirring reaction is carried out for 0.5 to 8 hours under the room temperature, then NaOH or KOH is added, the stirring reaction is carried out again for 0.5 to 3 hours under the room temperature, after that, the glucal can be generated. The synthetic method of glucal is also called as a one-pot synthetic method of the glucal and has the advantages of simple operation, shortened process flow, high yield, short reaction time, low cost, less three wastes, small environmental pollution and easy industrialization.

The invention discloses a method for separating salbutamol in pig urine by using the SLE method, which comprises the following steps: Step 1: sample pretreatment; collect pig urine, first add β-glucuronidase / arylsulfatase to enzymatically After enzymatic hydrolysis, add trichloroacetic acid to precipitate protein in pig urine, add phosphate buffer solution with 4 times the volume of pig urine with a pH range of 6.5 to 7.0, mix with a vortex mixer and centrifuge; take the supernatant after centrifugation; Step 2: After adding the supernatant to the SLE column, let it stand for 2 to 4 minutes; Step 3: Use the binary eluent to elute the SLE column at least twice, receive the eluate, and obtain the eluate containing albuterol . The object of the present invention is to provide a kind of method that adopts SLE method to separate albuterol in pig urine with high separation efficiency, simple operation and low detection limit.

A synthetic method of acetylated delta-hydroxy-alpha,beta-unsaturated furfural is disclosed. The method is characterized in that a glucal having a protective group, an organic solvent and water are mixed according to mole-volume ratio of 1 mol:50-250 L:0.6-2.8 L, a ring-opening reaction is performed by adopting FeCl3 as a catalyst, a product is mixed with triethylamine, DMAP and acetic anhydride according to a molar ratio of 1:1-3:0.1-0.5:0.5-3.0, the mixture is subjected to acetaylation at 0-45 DEG C, and neutralization, extraction and purification are performed after the reaction is finishedto obtain acetylated delta-hydroxy-alpha,beta-unsaturated furfural having different protective groups. Compared with the prior art, the method has characteristics of a simple process, convenient operation, nontoxic and economical agents, mild reaction conditions and a high reaction speed and a high yield, and is a green, economical and efficient novel acetylated Perlin aldehyde synthetic method having a good application prospect.

The present invention provides an application of glucal and a glucal derivative in preparation of drugs, specifically an application of the glucal and the glucal derivative in preparation of blood glucose reducing drugs, antiviral drugs, wound repairing drugs, anti-tumor drugs or anti-aging drugs. The glucal and the glucal derivative of the present invention comprise D-glucal and triacetylglucal. According to the present invention, with determinations by animal tests and in vitro tests, the results show that: the glucal and the glucal derivative have effects of blood glucose reducing, virus resistance, wound repairing, tumor resistance or aging resistance. The drugs of the present invention are oral tablets, capsules, oral solutions or granules or transdermic absorption injections or transdermic absorption patches, wherein the oral tablets, the capsules, the oral solutions or the granules or the transdermic absorption injections or the transdermic absorption patches are prepared by the glucal or the glucal derivative and a conventional pharmaceutic adjuvant according to a conventional method, the glucal or the glucal derivative is adopted as the active ingredient. The glucal and the glucal derivative of the present invention have great practical values in the field of medicine.

The invention discloses a preparation method of 4,6-O-benzylene-3-O-acetyl-D-glucal, comprising the following step: carrying out reduction reaction on a compound 11 in an organic solvent in the presence of complex of vanadium, acetic acid, zinc and ammonium salt, wherein the molar ratio of the acetic acid to the compound 11 is 0.1:1-20:1, the complex of vanadium is a complex of vanadium represented by formula 12 and / or formula 13, and the ammonium salt is ammonium chloride and / or ammonium bromide. The method has simple operation, avoids the usage of toxic reagents, has the advantages of low environmental pollution, mild reaction conditions, and high yield, and is suitable for industrial large-scale production.