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82results about How to "The reaction conditions are mild and safe" patented technology

Method for visible light catalytic synthesis of 3-sulfuryl spiro-trienone compound

The invention relates to a method for visible light catalytic synthesis of a 3-sulfuryl spiro-trienone compound. The method comprises dissolving N-aryl propiolamide and sulfinic acid as raw materials in an acetonitrile / water mixed solvent, adding water soluble eosin as a photocatalyst into the solution, carrying out irradiation on the mixed solution under a 3W blue LED visible light lamp for a reaction at the room temperature for 6-24h, and after the reaction, separating and purifying the crude product to obtain the 3-sulfuryl spiro-trienone compound. The method utilizes a visible light energy source, a simple and easy available sulfinic acid as a sulfone source, cheap water soluble eosin as a photocatalyst and air as an oxidant, realizes synthesis of the 3-sulfuryl spiro-trienone compound at the room temperature, greatly reduces the energy consumption, effectively prevents the use of metal catalysts and peroxide oxidants and has good reaction safety.
Owner:QUFU NORMAL UNIV

Preparation method of peramivir

InactiveCN102633686APrecise and controllable dosageHigh yieldOrganic chemistryOrganic compound preparationAntiviral drugKetone
The invention discloses a preparation method of an antiviral drug of peramivir, which is characterized in that 2-diazabicyclo [2.2.1] hept-5-en-3-one is used as an initial raw material for peramivir synthesis, and the overall yield is up to 35%. Compared with the prior art, the method has the advantages of high yield, fewer 'three wastes', safe and convenient operations, high purity of the obtained finished products, easy realization of industrial production, and the like.
Owner:FUAN PHARM (GRP) CO LTD

Nanometer microcrystalline cellulose reinforcing polylactic acid glycolic acid electrospun membrane, preparation method thereof and application

The invention discloses a nanometer microcrystalline cellulose reinforcing polylactic acid glycolic acid electrospun membrane, a preparation method thereof and application and relates to the field of biomedicine. Two natural organic polymer materials of PLGA and CNCs are composited, the method of preparing the electrospun film through electrospinning can effectively enhance the strength and the bioactivity of the materials, give full play to the biological nanometer effect and effectively compensate for the limitation of pure PLGA in biomedical application, and wound healing is well facilitated. In addition, the CNCs reinforcing PLGA electrospun membrane prepared through the method can also be used in fields of medicine controlled slow-release, repair of organs, such as skin, nerve and heart, tissue regeneration and the like.
Owner:BEOGENE BIOTECH GUANGZHOU

Method of zyme catalyzing cyclo-olefin oxidation

The invention relates to a method of enzyme catalyzing olefin expoxidation. In the aqueous solution, the bromine peroxidase is applied for biological catalyst and hydrogen peroxide or oxygen is taken as oxygen source to oxidate the olefin into expoxidation. Take the cyclohexen as example. The hydrogen peroxide is applied as the source. They react under the 20 DEG C. to 70 DEG C. for two to ten hours. The yield of epoxy cyclohexane to the hydrogen peroxide is more than 50 per cent and the selectivity of the epoxy cyclohexane is more than 85 per cent. After the reaction, the water phase is separated from the organic phase automatically, and the enzymes left in the water phase can be recycled. Boasting easy technical process, recycled enzymes and easy yield separation, the method is an environment-friendly green chemical process.
Owner:DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI

Method for synthesizing 2, 3-dimethyl-4-fluorophenol

The invention discloses a method for synthesizing 2,3-dimethyl-4-fluorophenol. The method comprises the following steps: adding aluminum trichloride in 2,3-dimethylfluorobenzene at a normal temperature and carrying out bromination reaction to obtain 3-bromo-6-dimethylbenzene; carrying out methoxylation on the 3-bromo-6-dimethylbenzene under the effect of N,N-dimethylformamide and sodium methoxideto obtain 3-methoxyl-6-dimethylbenzene; and carrying out hydrolysis on the 3-methoxyl-6-dimethylbenzene to obtain 2,3-dimethyl-4-fluorophenol. According to the synthesizing method, the 2,3-dimethylfluorobenzene which is low in price is used as a reaction raw material, in every step of reaction, an intermediate which is high in purity can be obtained to a maximum extent, thus, the total yield of total reaction is high, the purity of the final product reach up to 98% or above, the economic benefit is quite obvious, and the method is particularly suitable for industrial large-scale application and popularization.
Owner:SHANGHAI SINOFLUORO SCI

Biomimetic preparation method of strontium carbonate crystal

The invention discloses a biomimetic preparation method of a strontium carbonate crystal, wherein a coronary strontium carbonate nano crystal is prepared by a biomimetic method in a specific communication device by adopting strontium chloride hexahydrate and ammonium bicarbonate as reactants and sesbania gum as a biological regulation agent. According to the target product coronary strontium carbonate nano crystal, the corolla diameter is 3,000-6,000nm; the corolla is composed of nano rods with diameter being 50-80nm; the corolla structure is tight, with purity being greater than or equal to 99% and yield being 97-99%. The method disclosed by the invention has the characteristics of mild conditions, low energy consumption, large corolla diameter, tight corolla structure, high purity, highyield, low preparation cost, etc.
Owner:NANCHANG HANGKONG UNIVERSITY

Composite steel slag-based heavy metal adsorbent

The invention belongs to the technical field of water treatment, and particularly relates to a composite steel slag-based heavy metal adsorbent. The composite steel slag-based heavy metal adsorbent isused for removing heavy metal ion pollutants in water. The heavy metal adsorbent comprises, by weight, 60-70 parts of steel slag, 5-10 parts of straws, 15-25 parts of furnace ash and 5-10 parts of anadhesive. The adsorbent can be used for removing heavy metals in water bodies such as rivers, lakes and factory wastewater.
Owner:BAOSHAN IRON & STEEL CO LTD

Method for synthesizing (S)-2-aminobutanol

The invention provides a method for synthesizing (S)-2-aminobutanol. The method sequentially comprises steps as follows: (1) a supported metal catalyst is prepared; (2), (S)-2-aminobutanol is dissolved in deionized water, the pH (potential of hydrogen) value is adjusted to be 1-5, and the supported metal catalyst is added; hydrogen is introduced, the reaction temperature is controlled in the range from 60 DEG C to 70 DEG C, the reaction pressure is 2-4 MPa, and the mixture continuously reacts for 4-10 hours in the hydrogen atmosphere until hydrogen absorption stops; (3) after the reaction ends, the catalyst is separated from a reaction liquid, and a finished product (S)-2-aminobutanol is obtained through aftertreatment of filtrate. The method is low in production cost and simple and convenient to operate, raw materials are simple and easy to obtain, little pollution is caused to the environment, the operation is safety, the production yield is high, and the product quality is stable.
Owner:JIANGXI XIANKANG PHARMA CO LTD

Preparation method of 2,6-dihydroxytoluene

The invention discloses a preparation method of 2,6-dihydroxytoluene. The preparation method comprises the following steps of dissolving prepared 3,5-diamino-4-methylbenzoic acid in water, adding dilute sulphuric acid, stirring uniformly, adding ZnCl2, reducing the temperature to minus -2 to 2 DEG C after stirring uniformly, dropwise adding a sodium nitrite solution into the mixture, continuouslystirring to react for 5-6 hours after the dropwise adding is finished, then adding water and dilute sulphuric acid, mixing uniformly, then heating for boiling, reacting for 30-45 minutes, then addingsodium hydroxide, carrying out reflux reaction for 1-2 hours, cooling to room temperature, adding diethyl ether, stirring for 20-40 minutes, then adding zeolite, stirring and mixing for 1-2 hours, carrying out reduced-pressure distillation after filtering, and preparing the 2,6-dihydroxytoluene. The preparation method disclosed by the invention has the beneficial effects that the raw-material costis low, the operation is simple, safe and reliable, the requirements for the environmental conditions are mild, the product purity is high and the yield is high.
Owner:SUZHOU GAIDE FINE MATERIALS CO LTD

Th-MOF loaded Cu-based single-site catalytic material as well as preparation method and application thereof

The invention discloses a Th-MOF loaded Cu-based single-site catalytic material as well as a preparation method and application thereof. The invention belongs to the field of catalytic materials. The invention aims to solve the technical problem that an existing catalyst is low in catalytic activity. The catalytic material is composed of a single-site Cu and a Th-MOF material, the Th-MOF material is Th-BPYDC, the Th-MOF material is of a regular octahedron structure, and the space site group is Fm3m. The method comprises the steps of 1, preparing a Th-MOF material; 2, preparing a precursor solution containing copper ions; and 3, preparing the Th-MOF loaded Cu-based single-site catalytic material. The invention also relates to application of the Th-MOF loaded Cu-based single-site catalytic material in an electro-reduction NO3-ammonia synthesis reaction. The obtained catalytic material can achieve an ammonia generation rate up to 225.3 [mu] mol.h<-1 >.cm <-2 > and a Faraday efficiency of 92.5%.
Owner:EAST CHINA UNIV OF TECH

Charge-controllable polymer material as well as preparation method and application thereof

The invention provides a charge-controllable polymer material as well as a preparation method and application thereof. The polymer material is synthesized from dopamine and 5-hydroxytryptamine. The preparation method of the material comprises the following steps of: adding dopamine and a 5-hydroxytryptamine hydrochloride solution into a stirred alcohol ammonia solution according to a certain ratio, and stirring for 24 hours at room temperature in a dark place to form the polymer material. The polymer material has the advantages of excellent adhesion, secondary modification, charge controllability and the like, can be used for surface modification of most materials or directly used for drug delivery, and has a huge application prospect in many fields.
Owner:CENT SOUTH UNIV

Cordycepin/O-carboxymethyl chitosan nanoparticle and preparation method thereof

The invention discloses a cordycepin / O-carboxymethyl chitosan nanoparticle and a preparation method thereof. The grain size of the cordycepin / O-carboxymethyl chitosan nanoparticle is 100-200nm. The preparation method for the cordycepin / O-carboxymethyl chitosan nanoparticle comprises the following steps: dispersing cordycepin into a sodium chloride solution containing O-carboxymethyl chitosan; adding a sodium tripolyphosphate solution into the system; centrifuging, washing and vacuum-drying, thereby acquiring the cordycepin / O-carboxymethyl chitosan nanoparticle. According to the invention, the cordycepin / O-carboxymethyl chitosan nanoparticle prepared in the manner of using the O-carboxymethyl chitosan as a cordycepin nano-drug carrier, using sodium tripolyphosphate as a cross-linking agent and adopting an ionic cross-linking method is characterized by small grain size, uniform distribution, higher drug loading capacity and excellent slow release performance. The method disclosed by the invention is under mild and safe reaction conditions, uses no acid-base or organic solvent and is high in operability.
Owner:SHIJIAZHUANG ZANGNUO BIOTECH

Coumarin derivative and preparation and application thereof

The invention discloses a coumarin derivative and preparation and application thereof. 7-hydroxy-4-methyl coumarin as a raw material is subjected to substitution reactions with halogenated ethyl alcohol and 4-vinylbenzyl chloride in sequence, and then 7-[2-(4-vinyl benzyloxy)-ethyoxyl]-4-methyl coumarin is obtained. The method has the advantages that the operation is simple, the conditions are mild, the product is easy to purify, and the yield is high, the coumarin derivative synthesized by using the method has polymerizable double-bond elements, alkoxy flexible spacers and coumarin photosensitive groups, and when the coumarin derivative as a photosensitive monomer used for synthesis of a photostimulation response polymer material, the polymerization efficiency can be obviously improved. The water solubility and the degradability of the polymer material synthesized by using the counmarin derivative can be improved, the hydrophily and the hydrophobicity of the polymer material are moreeasily regulated and controlled, and therefore, in the use process of the polymer material as a drug carrier, the drug encapsulation and release rates can be better controlled.
Owner:CENT SOUTH UNIV

Method for removing oxime through catalysis of tellurium

The invention provides a method for removing oxime through catalysis of tellurium and relates to the technical field of oxime removal. According to the method provided by the invention, commercializeddiphenyl ditelluride ether is used as a catalyst; oxygen gas is used as an oxidant under a solvent-free condition and oxime is heated so that oxime can be removed to obtain a carbonyl compound; the catalyst also can be repeatedly utilized. The method is clean and environmentally friendly, low in cost and safe to operate, so that the method is an effective oxime removing method. According to the method provided by the invention, raw materials are selected from various aryl or alkyl substituted oxime. According to the method provided by the invention, reaction does not need a solvent so that the reaction cost can be reduced and a process is clean and environmentally friendly. The oxidant provided by the invention is the oxygen gas and can be used for sufficiently oxidizing a substrate, andthe yield is the highest.
Owner:YANGZHOU UNIV

Process for preparing 2,4-difluorocyanobenzene

The invention discloses a manufacturing method of 2, 4-difluocyanobenzene, which comprises the following steps: adopting N, N-dimethylacetamide as reacting solvent and 0.1-5% palladium complex as catalyst; making 0.5-2% alkaline metal carbonate as alkaline; reacting 2, 4-difluobromobenzene and ferrocyanide with molar rate at 1: 0.15-0.3 to react under 100-150 Deg C for 1-6h; filtering; decompressing the filtrate; fractioning to obtain the product. The invention shortens reacting flow path, which is simple to feed and dispose without poison in the whole course.
Owner:ZHEJIANG UNIV

Preparation method of 2-azanoradamantane-N-Oxyl

The invention discloses a preparation method of 2-azanoradamantane-N-Oxyl (Nor-AZADO). The method comprises the following steps: placing acetonedicarboxylic acid, glutaraldehyde and benzylamine in an aqueous hydrophosphate solution, and carrying out condensation and decondensation to obtain 9-benzyl-9-azabicyalo-[3,3,1]-nonyl-3-one; carrying out condensation dehydration on 9-benzyl-9-azabicyalo-[3,3,1]-nonyl-3-one and benzene or benzene ring substituted sulfohydrazide, and adding an alkali to obtain 2-(9-benzyl-9-azabicyalo-[3,3,1]-nonane-3-ylidene)-1-benzene or benzene ring substituted sulfohydrazide sodium / potassium salt; carrying out refluxing ring closing on the 2-(9-benzyl-9-azabicyalo-[3,3,1]-nonane-3-ylidene)-1-benzene or benzene ring substituted sulfohydrazide sodium / potassium salt in an organic solvent to obtain N-benzyl-2-azanoradamantane; debenzylating N-benzyl-2-azanoradamantane to obtain 2-azanoradamantane; and oxidizing 2-azanoradamantane by a peroxide oxidant to obtain the Nor-AZADO. The preparation method has the advantages of great increase of the synthesis yield, greenness and environmental protection, high efficiency, low cost, and easiness in industrial large-scale production.
Owner:深圳市宏辉浩医药科技有限公司

Preparation process of intermediate 2-cyanpyrazine of pyrazinamide drug

The invention discloses a manufacturing technique of 2-cyano pyrazine as pyrazine amide medicinal intermediate, which comprises the following steps: adopting N, N-dimethyl acetamide as reacting solvent and 0.1-5% palladium complex as catalyst; making 0.5-2% alkaline metal carbonate as alkaline; reacting 2-cyano pyrazine and alkaline metal ferrocyanide with molar rate at 1: 0.15-0.3 protected by nitrogen under 100-150 Deg C for 1-6h; filtering; decompressing the filtrate; fractioning to obtain the 2-cyano pyrazine. The invention shortens reacting flow path, which is easy to feed and dispose without poison in the whole course.
Owner:ZHEJIANG UNIV

Method for continuously preparing 1-(methylsulfonyl)-2-(phenyl ethynyl) benzene by adopting electrochemical micro-channel

The invention discloses a method for continuously preparing 1-(methylsulfonyl)-2-(phenyl ethynyl) benzene by adopting an electrochemical micro-channel, which comprises the steps of dissolving methyl(2-(phenylethynyl) phenyl) thiane shown as a formula I in the description and an electrolyte in a solvent to obtain a homogeneous solution; and pumping the homogeneous solution into an electrochemical micro-channel reaction device, and carrying out an electrolytic reaction to obtain a reaction solution containing 1-(methylsulfonyl)-2-(phenyl ethynyl) benzene as shown in a formula II in the description. Compared with the prior art, the electrochemical micro-channel reaction device is adopted, the reaction time is short, the yield of reaction products is high, and the reaction efficiency is remarkably improved. Meanwhile, expensive metal catalysts or oxidizing agents do not need to be added, and the method is low in cost, easy and convenient to operate, environmentally friendly and green.
Owner:CHINA PHARM UNIV

Modification method of activated carbon fiber material

The invention discloses a modification method of an activated carbon fiber material. The method adopts polyacrylonitrile-based activated carbon fiber as a raw material, adopts a modification reagent soaking and heat treatment method to carry out composite modification, and prepares modified activated carbon fiber cloth through soaking, heat treatment, drying and other methods. According to the modification method, the adsorption capacity of the activated carbon fibers to pollution gas such as SO2 is further improved, finally, the activated carbon fiber cloth with excellent performance is prepared and serves as an insertion piece material of a mask, the performance of the mask for filtering poisonous and harmful gas such as SO2 and NOx is effectively improved, modification conditions are mild and environmentally friendly, the modified material is low in cost, and the product can better improve the life of people and meet the requirements of the public.
Owner:NANCHANG NORMAL UNIV

A kind of synthetic route and preparation method of irbesartan

The invention relates to a synthetic route and a preparation method of irbesartan. The method comprises three steps: (1) reacting a compound I (2-cyano-4'-methyl diphenyl), an inorganic salt oxidant, and an inorganic salt reductant in dichloromethane and water to form a compound IRB-02 (2-cyano-4'-bromomethylbiphenyl); (2) reacting a compound IRB-02, a compound IRB-01 (2-butyl-1, 3-diaza spiro [4.4] nonane-1-vinyl-4-ketone hydrochloride), tetrabutylammonium bromide and inorganic alkali in dichloromethane and water to obtain a compound IRB-03 (2-butyl-3-[(2-cyano biphenyl-4-base)methyl]-1,3-diaza spiro [4.4] nonane-1-vinyl-4-ketone); and (3) reacting a compound IRB-03, tetrabutylammonium bromide, zinc chloride and sodium azide in toluene to obtain the irbesartan.
Owner:珠海保税区丽珠合成制药有限公司

Synthesis method for 1-ethyl-3-(3-dimethyl amino propyl)-carbonized diimine A iodate

The invention discloses a synthesis method for 1-ethyl-3-(3-dimethyl amino propyl)-carbonized diimine A iodate. The synthesis method comprises the following steps of (1) adding 1-ethyl-3-(3-dimethyl amino propyl)-carbonized diimine into a halohydrocarbon solvent, uniformly stirring the two materials, and cooling to be lower than 15 DEG C to obtain a solution A; (2) adding iodomethane into the solution A obtained in the step (1), controlling the temperature at lower than 25 DEG C for generating reaction, and obtaining a reaction solution B after the reaction is completely executed; (3) adding a hydrocarbon solvent into the reaction solution B obtained in the step (2) for crystallization, and collecting and drying crystallized solids to obtain the 1-ethyl-3-(3-dimethyl amino propyl)-carbonized diimine A iodate. According to the synthesis method, the 1-ethyl-3-(3-dimethyl amino propyl)-carbonized diimine A iodate is obtained in a higher-yield way by selecting the proper solvent and controlling the temperature; the product is crystallized in a higher-purity way through the specific solvent; the synthesis method is convenient to operate and suitable for large-scale production.
Owner:ZHEJIANG BULK CHEM

Method for preparing ammonium manganese phosphate crystal

The invention discloses a method for preparing ammonium manganese phosphate crystal. Manganese chloride or manganese sulfate is used as a manganese source reactant, ammonium phosphate is used as a phosphorus source reactant, and starch is used as a biological regulating agent to prepare the ammonium manganese phosphate crystal. The method comprises the following steps: sequentially adding manganese chloride or manganese sulfate, ammonium phosphate, and a mixture solution of starch and ammonium chloride or ammonium sulfate into a communicating reactor provided with left and right ear grooves and left, middle and right baffles, and filtering, washing and drying a product after the reaction is finished to obtain the ammonium manganese phosphate crystal. The purity of the prepared ammonium manganese phosphate crystal reaches 99.0%-99.9%, the yield reaches 95%-97%, the purity and crystallinity are high, and the method has the advantages of being simple in process, mild in reaction condition, low in energy consumption and cost and the like.
Owner:NANCHANG HANGKONG UNIVERSITY

Preparation method of cyclopropane compounds

The invention discloses a preparation method of cyclopropane compounds. The structural formula of the cyclopropane compounds is shown in a formula I. According to the preparation method, olefins shown as a formula II have cyclopropanation reaction under the actions of a methylene transfer agent and an additive to generate cyclopropane compounds shown as the formula I, wherein the methylene transfer agent is a mixture of diethylzinc and diiodomethane, and the additive is a mixture of acid and ether. According to the preparation method provided by the invention, olefins with different structures are taken as substrates, and the mixture of diethylzinc solution and diiodomethane is taken as the methylene agent, so that the cyclopropane compounds are finally obtained with high yield under the synergistic effect of catalytic amount of trichloroacetic acid and equivalent amount of 1, 2-dimethoxyethane. The preparation method is mild and safe in reaction conditions, easy for large-scale operation, wide in the using range of the substrates and high in yield and has great industrialization potential.
Owner:INST OF CHEM CHINESE ACAD OF SCI

Preparation method of 4-methyl-2-pentanol

The invention discloses a preparation method of 4-methyl-2-pentanol. The preparation method comprises the following steps of: adding mesityl oxide into a hydrogenation kettle; adding a nickel-containing three-way catalyst; introducing hydrogen while performing stirring; carrying out a catalytic hydrogenation reaction; performing filtering to remove the catalyst after the reaction; and carrying out distillation separation on filtrate to obtain the 4-methyl-2-pentanol. The method has the advantages of milder and safer reaction conditions, simplicity and convenience in operation, high yield, low cost, good quality and the like, and has a wide application prospect.
Owner:SUZHOU JINGYE MEDICINE & CHEM

A kind of preparation method of 3,4-methylenedioxyphenol

The invention discloses a preparation method of 3,4-methylenedioxyphenol, which is characterized in that 3,4-methylenedioxyacetophenone is used as a starting material, and is added dropwise in toluene and formic acid solution Hydrogen peroxide undergoes an oxidation reaction, and the resulting substance is hydrolyzed, neutralized, and rectified to obtain the target product of 3,4-methylenedioxyphenol. The invention has the advantages of easy-to-obtain raw materials, mild and safe reaction conditions, simple and convenient operation, good product purity and high yield.
Owner:SUZHOU JINGYE MEDICINE & CHEM

A kind of synthetic method of 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide methyl iodide salt

The invention discloses a synthesis method for 1-ethyl-3-(3-dimethyl amino propyl)-carbonized diimine A iodate. The synthesis method comprises the following steps of (1) adding 1-ethyl-3-(3-dimethyl amino propyl)-carbonized diimine into a halohydrocarbon solvent, uniformly stirring the two materials, and cooling to be lower than 15 DEG C to obtain a solution A; (2) adding iodomethane into the solution A obtained in the step (1), controlling the temperature at lower than 25 DEG C for generating reaction, and obtaining a reaction solution B after the reaction is completely executed; (3) adding a hydrocarbon solvent into the reaction solution B obtained in the step (2) for crystallization, and collecting and drying crystallized solids to obtain the 1-ethyl-3-(3-dimethyl amino propyl)-carbonized diimine A iodate. According to the synthesis method, the 1-ethyl-3-(3-dimethyl amino propyl)-carbonized diimine A iodate is obtained in a higher-yield way by selecting the proper solvent and controlling the temperature; the product is crystallized in a higher-purity way through the specific solvent; the synthesis method is convenient to operate and suitable for large-scale production.
Owner:ZHEJIANG BULK CHEM

Polymer material entrapping glucose oxidase and preparation method and application of polymer material

The invention provides a polymer material entrapping glucose oxidase and a preparation method and application of the polymer material. The polymer material is a polydopamine nanocage composed of polydopamine. According to the polymer material, first a nano nano-coordination polymer is formed through folic acid-zinc chloride coordination to entrap glucose oxidase, then dopamine is oxidized and self-polymerized on the surface of the nano-coordination polymer to form a polydopamine shell, and finally the nano-coordination polymer is dissociated to obtain the polymer material. The invention provides a self-polymerizing nano cage carrier, the preparation steps are simple, the carrier with stable particle size, capable of effectively maintaining the activity of biological enzymes under physiological conditions and delivering protein drugs is obtained, and the high-efficiency delivery is achieved and the biological active is maintained.
Owner:HUNAN PROVINCIAL TUMOR HOSPITAL
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