55 results about "Glucal" patented technology

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 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 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 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 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 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.

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.