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31results about How to "Many side effects" patented technology

Method for synthesizing triallyl phosphate

The invention provides a method for synthesizing triallyl phosphate, and belongs to the technical field of compound synthesis. The method comprises the following steps: adding allyl alcohol serving as a raw material and an acid-binding agent into a solvent under protection of nitrogen; then, adding phosphorus oxychloride to react; pumping and filtering the reacting liquid; washing, drying, decoloring and concentrating to obtain triallyl phosphate; controlling the reacting temperature to be less than negative 30 DEG C when the phosphorus oxychloride is dropwise added for 3.4-7.5 hours; and naturally heating to -2-zero DEG C, and stopping reaction. The synthesizing method is simple and easy to operate, and the prepared triallyl phosphate has high yield and high purity.
Owner:SHIJIAZHUANG SAN TAI CHEM CO LTD

Method for producing 4-propyl-[1,3,2]dioxathiolane-2,2-dioxide

A method for producing 4-propyl-[1,3,2]dioxathiolane-2,2-dioxide comprises an addition reaction, an oxidation reaction and a purifying process. The method concretely comprises the following steps: 1, carrying out the addition reaction: carrying out addition reaction on thionyl chloride and 1,2-pentanediol as reaction raw materials; 2, carrying out the oxidation reaction: adding a sodium hypochlorite and catalyst mixed solution, carrying out the oxidation reaction to obtain a water phase and organic phase co-existence reaction solution, standing the water phase and organic phase co-existence reaction solution for layering, and separating the obtained water phase to obtain the organic phase which is crude 4-propyl-[1,3,2]dioxathiolane-2,2-dioxide; and 3, purifying: carrying out molecular distillation to obtain 4-propyl-[1,3,2]dioxathiolane-2,2-dioxide. The purity of the prepared 4-propyl-[1,3,2]dioxathiolane-2,2-dioxide can be greater than 99.5%, the water content is not greater than 100PPM, the acid value is not greater than 100PPM, and 4-propyl-[1,3,2]dioxathiolane-2,2-dioxide can be added to a battery in order to improve the performances of the battery and prolong the life of the battery.
Owner:SHIJIAZHUANG SAN TAI CHEM CO LTD

Method for preparing hexafluorobutadiene from iodine and chlorine

The invention relates to a method for preparing hexafluorobutadiene from iodine and chlorine. The method comprises the following steps: preparing a metal coordinated ionic liquid solvent, and reacting iodine with chlorine to prepare iodine monochloride; reacting iodine monochloride with chlorotrifluoroethylene in the presence of the metal coordinated ionic liquid solvent to prepare 1,2-dichloro-2-iodo-1,1,2-trifluoroethane; carrying out a reaction on the 1,2-dichloro-2-iodo-1,1,2-trifluoroethane in the presence of the metal coordinated ionic liquid solvent under the catalysis of zinc powder to obtain 1,2,3,4-tetrachloro-1,1,2,3,4,4-hexafluorobutane; and reacting the 1,2,3,4-tetrachloro-1,1,2,3,4,4-hexafluorobutane with zinc powder in the presence of the metal coordinated ionic liquid solvent to generate hexafluorobutadiene.
Owner:ZHEJIANG BRITECH CO LTD

Method for preparing electronic grade gallic acid

The invention discloses a method for preparing electronic grade gallic acid by using Tara powder as raw material and combining microorganism fermentation method with resin absorption. The method comprises the following steps: fermenting Tara powder with aspergillus niger to prepare raw gallic acid, decoloring the raw gallic acid in ethanol solution, filtrating to obtain filtrate, sending the filtrate through a anionic-cationic exchange resin column, performing reduced pressure evaporation to recycle ethanol until precipitating crystals, cooling, filtrating to obtain refined gallic acid and performing vacuum drying to obtain the electronic grade gallic acid. The contents of Na, Fe, K, Ca, Mg, Cu, Zn, Al and Mn ions are not more than 50ppb. The method has no pollution, high yield and low cost, the resin can be recycled and the method does not damage resin and is applicable to preparing detergent used to wash integrated circuits in electronic industry.
Owner:先微康新材料科技有限公司

Preparation method of antiviral drug tenofovir disoproxil fumarate intermediate chloromethyl isopropyl carbonate

The invention discloses a preparation method of antiviral drug tenofovir disoproxil fumarate intermediate chloromethyl isopropyl carbonate, and belongs to the field of antiviral chemical drugs. The preparation method is characterized in that methyl formate as a raw material is synthesized into chloromethyl chloroformate by an one-kettle method and the chloromethyl chloroformate undergoes an esterification reaction to form chloromethyl isopropyl carbonate. The preparation method is easy for operation, has a low cost and a high yield, realizes high purity of products, and is very suitable for industrialized production.
Owner:扬州三友合成化工有限公司

Furfural preparation process

The invention discloses a furfural preparation process. The furfural preparation method adopts a two-step method. The method comprises the following specific steps: firstly, catalyzing hydrolysis of hemicellulose in corncobs by adopting an SO4 < 2-> / Fe2O3-alpha-Al2O3 supported solid acid catalyst; then catalyzing corncob hydrolysis reaction liquid to prepare furfural by using a novel catalyst instead of sulfuric acid, stripping crude aldehyde in the reaction system by using nitrogen instead of water vapor, performing alkali washing and refining on the stripped crude aldehyde by using a continuous centrifugal extraction refining method, introducing the crude aldehyde into a rectifying tower, and rectifying to obtain furfural with the purity of over 99%. According to the method, the furfuralis prepared through the two-step method, lignin and cellulose in the corncob residues can be reserved for reuse, the concentration of the crude aldehyde is increased through nitrogen steam stripping,the furfural production yield is increased, and the wastewater yield is reduced.
Owner:QINGDAO UNIV OF SCI & TECH

Method for synthesizing triallyl phosphite

The invention discloses a method for synthesizing triallyl phosphite, and belongs to the field of technologies for synthesizing compounds. The method includes adding allyl alcohol and acid binding agents into solvents under the protection of nitrogen, then adding phosphorus trichloride into the solvents and carrying out reaction to obtain reaction liquid; carrying out suction filtration on the reaction liquid and washing, drying, decolorizing and concentrating the reaction liquid to obtain the triallyl phosphite. The allyl alcohol is used as a raw material. The reaction temperatures are lower than -8 DEG C under the control when the phosphorus trichloride is dropwise added into the solvents for the dropwise adding time of 3-4 h, then the temperatures are naturally increased until the temperatures reach 0-30 DEG C, and heat-insulation treatment is carried out for 1-2 h. The method for synthesizing the triallyl phosphite has the advantages that the method is simple and is easy to implement, and the triallyl phosphite prepared by the aid of the method is high in yield and purity.
Owner:SHIJIAZHUANG SAN TAI CHEM CO LTD

Preparation method of palbociclib parent nucleus structure compound

The invention provides a preparation method of a palbociclib mother nucleus structure compound. The preparation method comprises the following step: preparing the palbociclib parent nucleus structurecompound as shown in a formula (I) which is described in the specification by taking cytosine or an intermediate 1 or an intermediate 2 as a starting raw material, wherein the intermediate 1 and the intermediate 2 are as described in the specification, and X is selected from halogen. The method is wide in the source of the starting material, simple in operation process, less in side reaction and high in purity, and accords with the concept of modern green industrial production.
Owner:SHANDONG MAYOHUAWEI TECH CO LTD

N,N-dimethyl tetrahydrofurfuryl amine synthesis method

The invention relates to organic compound synthesis methods, in particular to an N,N-dimethyl tetrahydrofurfuryl amine synthesis method. The method includes steps: 1) mixing reactants with N,N-dimethyl formamide or N,N-dimethylacetamide and formic acid in a reaction vessel, and performing heating reaction; 1) after heating reaction is finished, performing distillation recovery of DMF (dimethyl formamide) or DMAC (dimethylacetamide) and the formic acid, and subjecting residues to vacuum distillation to obtain N,N-dimethyl furfuryl amine which is an intermediate product; 3) subjecting the intermediate product N,N-dimethyl furfuryl amine to catalytic hydrogenation, and distilling to obtain a product of N,N-dimethyl tetrahydrofurfuryl amine. The N,N-dimethyl tetrahydrofurfuryl amine synthesis method has advantages that raw materials are cheap and extensive in source; problems of low furfural yield and difficulty in separation due to instability of furfural acids are avoided, and acidity and reducibility of the formic acid are fully used; high hydrogenation selectivity and catalyst recyclability are realized; mild conditions, easiness in implementation and high raw material utilization rate are realized, and excessive formic acid and N,N-dimethyl formamide or N,N-dimethylacetamide are easy to recover.
Owner:XIAMEN UNIV

Novel photochromic azobenzene compound and synthesis method thereof

The invention provides a novel photochromic azobenzene compound and a synthesis method thereof and relates to a novel compound N-[4-[2-(4-methoxyphenyl) diazenyl] phenyl]-2-nitroaniline with a photochromic property and a synthesis method of the novel compound. The synthesis method comprises diazonium coupling reaction and coupling reaction between aromatic amine and aromatic halides. According to the invention, coupling reaction conditions of aromatic amine and aromatic halides are very simple, to be specific, only alkali metal fluorides with equal molar mass are added into reaction liquid, and reflux is carried out at 130 DEG for 3 h; a solvent is not required to be subjected to anhydrous anaerobic treatment, that reaction is carried out under nitrogen or argon atmosphere is not required, no side reaction is generated, aftertreatment of the product is simple, the conversion rate is higher, the yield of the target product is 48-74%, in addition, equipment adopted by the invention is relatively simple, the cost is low, and obvious economic benefits and environment-protection benefits are realized. The defects, in the prior art, that coupling reaction between aromatic amine and aromatic halides can be carried out at high temperature, with existence of inorganic base and under anhydrous anaerobic inert atmosphere usually, the reaction time is long, side reaction is multiple and the yield is low are overcome.
Owner:HUBEI UNIV

Method for removing perfluorinated compounds (PFCs) in wastewater through micro-nano gas-floating coupled electrooxidation device

The invention relates to a method for removing perfluorinated compounds (PFCs) in wastewater through a micro-nano gas-floating coupled electrooxidation device. The method comprises the steps that (S1)a water inlet pump and a micro-nano bubble generation device are started, the gas inlet amount is adjusted to be 0.3-0.7 mL / min, and a milky gas-water mixture reaches a contact chamber of a reactiondevice through a high-speed water outlet diffuser; (S2) a stirrer is started, the pH value of the wastewater is adjusted through acid or base firstly through a chemical adding groove, and then a coagulant is added; (S3) the gas-water mixture reaches a separation chamber subsequently, the PFCs in the wastewater float upwards to the water surface under the effect of coercing and jacking of bubbles and the effect of a small amount of flocculant, and enter an electrooxidation unit from a slag-water mixture outlet, and the wastewater not containing the PFCs is discharged from a water outlet of a separation chamber; (S4) an electrolyte is added into the electrooxidation unit, after a collected PFCs water-slag mixture reaches a certain volume, the current density is adjusted for electrolysis, andpurified water is discharged from the water outlet; and (S5) the wastewater discharged from the water outlet finally enters a water outlet groove and is discharged after reaching the standard.
Owner:江苏智诚达环保科技有限公司

Method for synthesis of long-chain fatty acid ester derivative

The invention relates to a method for synthesis of a long-chain fatty acid ester derivative. Specifically, a hydrochloride of glycine methyl ester or glycine ethyl ester is used as a catalyst to catalyze the esterification reaction of long-chain fatty acid. The method includes: subjecting alcohol and long-chain fatty acid to esterification reaction under the action of the catalyst at certain temperature condition, then conducting extraction and precipitation with ethyl acetate, performing flushing with a sodium chloride aqueous solution for purification. A hydrochloride of glycine methyl esteror glycine ethyl ester is adopted as the catalyst, which belongs to a green catalyst, is the development trend of modern chemistry, has the characteristics of no corrosion to the reaction kettle, lowprice, no toxicity and the like, and is suitable for use as a catalyst to produce palmitate and laurate perfume raw materials.
Owner:PANASIA OLAUGHLIN BIO TECH WUHAN CO LTD

Enteral nutrition preparation containing konjac mannan oligosaccharide and L-glutamine and application

The invention belongs to the technical field of medicines, and particularly discloses an enteral nutrition preparation containing konjac mannan oligosaccharide and L-glutamine and application thereofin hyperlipoidemia nutritional therapy. When the method is adopted in the nutritional therapy of a hyperlipoidemia rat model, a certain curative effect is realized, no toxic and side effects exist, the preparation method is simple, the preparation raw materials are easy to obtain, and the application prospect is wide.
Owner:WUHAN GENERAL HOSPITAL OF GUANGZHOU MILITARY

Preparation method of N-formyl cefotaxime

The invention discloses a preparation method of N-formyl cefotaxime, which is characterized by comprising the following steps: adding anhydrous formic acid into acetic anhydride, controlling the temperature at 25-35 DEG C, reacting for 30 minutes, cooling to 15 DEG C, adding cefotaxime acid in batches, heating to 35-40 DEG C, adding a metal catalyst to continue reacting when reactants start to agglomerate, reacting for 30 minutes, adding purified water, and reacting for 30 minutes to obtain N-formyl cefotaxime. And adjusting the pH value when white crystals are separated out, filtering and washing when the temperature is reduced to 10-15 DEG C, and drying at the temperature of 50-60 DEG C and the pressure of-0.085--0.095 Mpa until the water content is less than 2.5% to obtain a target product. According to the method, multi-step synthesis by taking 7-ACA as a raw material is not needed, the production cost is effectively reduced, the reaction steps are simple, the steps of phase inversion purification, carbon decoloration and the like are not needed, the operation is simple and easy to control, the weight yield can reach 80%, and the highest product purity can reach 98.6%. The method fills the blank of N-formyl cefotaxime impurities prepared by chemical synthesis, and has important theoretical significance and practical application value for improving the quality of cefotaxime sodium and reducing the clinical medication risk.
Owner:河北合佳创新医药科技有限公司

Synthesizing method of 2-butyl-1-octanol

The invention discloses a synthesizing method of 2-butyl-1-octanol. The method includes the following steps of conducting an aldol condensation reaction with n-caproaldehyde as the initiator to obtain2-butyl-2-octenal, wherein a catalyst in the aldol condensation reaction is barium hydroxide; conducting a primary reduction reaction on 2-butyl-2-octenal to obtain a mixture of aldehyde and alcohol,and conducting a secondary reduction reaction on the mixture of aldehyde and alcohol to obtain 2-butyl-1-octanol, wherein a reducing agent in the primary reduction reaction is palladium on carbon, and a reducing agent in the secondary reduction reaction is sodium borohydride. The method is easy to operate, few byproducts are produced, yield is high, the requirements for devices are not high, andindustrial production is easy.
Owner:福建未来药业有限公司

Process for producing 7-amino-3-[(1-methyl pyrrolidine) methyl]-3- cephalosporin-4-carboxylic dihydrochloride

The invention discloses a method for preparing 7-amino-3-[(1-methylpyrro-lidinio)methyl]-3-cephem-4-carboxylic acid dihydrochloride, which comprises the following steps: imidazole, trimethylchlorosilane and 7-ACA react in a methylene dichloride solvent at a temperature of between 10 and 30 DEG C, and then are filtered; the temperature is reduced, and TMSI is dripped to react; THF is added into the mixture after methylene dichloride is distilled from a reaction feed liquid, and a N-methylpyrrolidine solution is dripped and stirred at a temperature of between 30 DEG C below zero and 25 DEG C below zero to react; methanol is dripped after the reaction, and then concentrated hydrochloric acid or hydriodic acid is dripped to hydrolyze; a hydrolysate is added with the methylene dichloride, and an aqueous phase is obtained through the separation; a yellow aqueous solution is obtained after the aqueous phase is decolored; and then acetone is added into the mixture to be filtered, washed and dried to obtain a 7-MPCA product. The methylene dichloride is distilled, so as to effectively improve the utilization rate of equipment, and the method can improve 30 percent of the utilization rate ofthe equipment compared with a process that the methylene dichloride is not distilled; and imidazole hydrochloride generated by the reaction which affects the subsequent layering and crystallization is filtered, which is favorable for the reaction, and ensures that the yield can reach 100 percent and the purity of a liquid phase is more than 99 percent.
Owner:河北九派制药股份有限公司

A kind of method of producing 4-propyl vinyl sulfate

A method for producing 4-propyl-[1,3,2]dioxathiolane-2,2-dioxide comprises an addition reaction, an oxidation reaction and a purifying process. The method concretely comprises the following steps: 1, carrying out the addition reaction: carrying out addition reaction on thionyl chloride and 1,2-pentanediol as reaction raw materials; 2, carrying out the oxidation reaction: adding a sodium hypochlorite and catalyst mixed solution, carrying out the oxidation reaction to obtain a water phase and organic phase co-existence reaction solution, standing the water phase and organic phase co-existence reaction solution for layering, and separating the obtained water phase to obtain the organic phase which is crude 4-propyl-[1,3,2]dioxathiolane-2,2-dioxide; and 3, purifying: carrying out molecular distillation to obtain 4-propyl-[1,3,2]dioxathiolane-2,2-dioxide. The purity of the prepared 4-propyl-[1,3,2]dioxathiolane-2,2-dioxide can be greater than 99.5%, the water content is not greater than 100PPM, the acid value is not greater than 100PPM, and 4-propyl-[1,3,2]dioxathiolane-2,2-dioxide can be added to a battery in order to improve the performances of the battery and prolong the life of the battery.
Owner:SHIJIAZHUANG SAN TAI CHEM CO LTD

A kind of n, n-dimethyltetrahydrofurfurylamine synthetic method

The invention relates to organic compound synthesis methods, in particular to an N,N-dimethyl tetrahydrofurfuryl amine synthesis method. The method includes steps: 1) mixing reactants with N,N-dimethyl formamide or N,N-dimethylacetamide and formic acid in a reaction vessel, and performing heating reaction; 1) after heating reaction is finished, performing distillation recovery of DMF (dimethyl formamide) or DMAC (dimethylacetamide) and the formic acid, and subjecting residues to vacuum distillation to obtain N,N-dimethyl furfuryl amine which is an intermediate product; 3) subjecting the intermediate product N,N-dimethyl furfuryl amine to catalytic hydrogenation, and distilling to obtain a product of N,N-dimethyl tetrahydrofurfuryl amine. The N,N-dimethyl tetrahydrofurfuryl amine synthesis method has advantages that raw materials are cheap and extensive in source; problems of low furfural yield and difficulty in separation due to instability of furfural acids are avoided, and acidity and reducibility of the formic acid are fully used; high hydrogenation selectivity and catalyst recyclability are realized; mild conditions, easiness in implementation and high raw material utilization rate are realized, and excessive formic acid and N,N-dimethyl formamide or N,N-dimethylacetamide are easy to recover.
Owner:XIAMEN UNIV

Traditional Chinese medicine composition for treating dysentery and preparing method thereof

The invention discloses a traditional Chinese medicine composition for treating dysentery. The traditional Chinese medicine composition is prepared from, by weight, 300-410 parts of ludwigia prostrate and 185-215 parts of radix sophorae flavescentis. The preparing method of the traditional Chinese medicine composition includes the following steps that 1, the raw materials are broken and mixed; 2, the mixed materials are decocted three times, the mixed materials are decocted for 2 h for the first time, for 1.5 h for the second time and for 1 h for the third time, and decoction is converged; 3, the decoction is filtered and concentrated to clear paste with the relative density of 1.08 at the temperature of 80 DEG C; 4, the clear paste is cooled, ethyl alcohol is added so that the alcohol content of the clear paste reaches 50-55%, the mixture is stirred uniformly and stands for 48 h, then supernate is taken and filtered, ethyl alcohol is recovered from filter liquor until alcohol smell is eliminated, and the filter liquor continues to be concentrated to clear paste with the relative density of 1.08 at the temperature of 80 DEG C; 5, the clear paste is dried in a belt type vacuum mode, smashed and granulated.
Owner:华润三九(郴州)制药有限公司
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