143 results about "Ethyl propiolate" patented technology

The invention relates to the technical field of lithium ion electrolytes, and in particular relates to a lithium-ion battery electrolyte with both high and low temperature performances. The electrolyte comprises lithium hexafluorophosphate, mixed organic solvents, filming additives, additives for improving the dielectric constant and the low temperature infiltration capability, and a lithium salt type additive, wherein the mixed organic solvents comprise a carbonic ester solvent and a linear carboxylic ester solvent; the linear carboxylic ester solvent in the mixed organic solvents is one or a mixture of more than two of ethyl propionate, propionic acid n-propyl ester, n-propyl acetate, acetic acid n-butyl ester and isobutyl acetate; and the additives for improving the dielectric constant and the low temperature infiltration capability are one or a mixture of more than two of fluoro ethylene carbonate, difluoro ethylene carbonate and 4-trifluoromethyl ethylene carbonate. A battery prepared from the lithium-ion battery electrolyte with both high and low temperature performances is long in service life, and both the good low temperature discharge performance of the battery is ensured, and the storage performance of the battery at the high temperature of 60 DEG C is effectively considered.

The invention provides a method for preparing furfuryl alcohol by utilizing a hydrogen transfer reaction to catalyze furfural. The method comprises the following steps that under the catalysis of a heterogeneous catalyst, namely magnetic hydroxyapatite, the furfural and alcoholic compounds with hydrogen donors are subjected to the hydrogen transfer reaction, wherein the ratio of the magnetic hydroxyapatite to the alcoholic compounds to the furfural is 20-120 g to 8-20 L to 1 mol. A reaction container is filled with nitrogen (N2) of which pressure is 1-20 bar at room temperature, the reaction temperature is 100 DEG C-200 DEG C, and a reduced product, namely the furfuryl alcohol, is obtained after 1-12 h. The method for preparing the furfuryl alcohol by utilizing the hydrogen transfer reaction to catalyze the furfural is simple in process, convenient to operate and safe and environmentally friendly. The catalyst is a non-precious metal catalyst and cheap and easy to obtain, has magnetism and is easy to separate, and can be reused repeatedly. The activity does not decrease. The industrial cost of preparing the furfuryl alcohol can be lowered to a large extent, ethyl levulinate can be catalyzed to react and gamma-valerolactone is generated, and other compounds containing C=O bonds can be also reduced.

The invention relates to a preparation method for quizalofop-p-ethyl, in particular to a method which uses p-hydroxybenzaldehyde to replace the raw material hydroquinone used in the traditional technology and react with S (-)-N-tosyl ethyl lactate to prepare R (+)-2-(p-oxy) propionate which is then reacted with 2,6- dichloro-quinoxaline to prepare high-purity quizalofop-p-ethyl through condensation.

The invention relates to a method for preparing ethyl levulinate based on catalysis of alcoholization of furfuryl alcohol with carbon-based solid acid, and relates to ethyl levulinate. The method comprises the following steps: uniformly mixing furfuryl alcohol, anhydrous ethanol and the carbon-based solid acid; adding a mixture obtained from the former step into a stainless steel high pressure reaction kettle; closing the reactor; and catalyzing the alcoholization of the furfuryl alcohol so as to prepare ethyl levulinate. The condition for catalysis of the alcoholization of the furfuryl alcohol is as follows: the reaction temperature is 100-150 DEG C, the stirring rotating speed is 300-500rpm, and the reaction time is 0.5-2.5 hours. The weight ratio of furfuryl alcohol to ethanol is (0.01-0.1):1, and the mass ratio of furfuryl alcohol to carbon-based solid acid is (1-4):1. The carbon-based solid acid can be hydrothermal carbon-based solid acid or carbonized carbon-based solid acid. The carbon-based solid acid is used as a catalyst which is simple to prepare and low in cost, and can be repeatedly used, so that the product yield is high and the byproducts are fewer. The method is simple in reaction system, mild in reaction condition, short in reaction time, environment-friendly, low in cost and convenient to posttreat.

The invention relates to a preparation method of pitavastatin calcium for treating hyperlipidemia. The preparation method comprises the following steps: performing cyclization on 2-amino-4'-fluorobenzophenone (III) and ethyl 3-cyclopropyl-3-oxo-propanoate (II), and then reducing with LiAlH4 to obtain 2-cyclopropyl-4-(4-fluorophenyl)-3-quinoline methanol (V); bromizing the V to obtain 2-cyclopropyl-3-bromomethyl-4-(4-fluorophenyl) quinoline (VI); reacting the VI with triphenylphosphine to obtain (2-cyclopropyl-4-(4-fluorophenyl)-quinoline-3-yl) methyltriphenylphosphonium bromide (VII), performing alkali treatment on a phosphonium salt, then forming phosphonium ylide, performing condensation with (3R, 5S)-6-oxo-3, 5-isopropylidene-dioxo-6-heptenoic acid tert-butyl ester (VIII) to obtain a compound IX; and acidifying the compound IX with hydrochloric acid, performing hydrolysis deprotection with sodium hydroxide, performing salt formation and purification with chiral amine and forming a calcium slat to obtain a final product. The whole route has reasonable design, the process flow is simple, starting raw materials and reagents used by the preparation method can be purchased from the market, the reagents with severe toxicity and serious pollution are not used in a reaction process, the post-treatment of an intermediate is simple, and the preparation method has the advantages of high yield and is easy to purify.

The invention discloses a manganese compound and a preparation method and application thereof, and relates to the technical field of magnetic resonance imaging (MRI). The manganese compound is dichloro-N-(2-propionic carbethoxy)-N,N-bis(2-picolyl) amine synthetic manganese, and the molecular formula is C17H21Cl2MnN3O2. The preparation method for the manganese compound comprises the following steps: dissolving ligand dichloro-N-(2-propionic carbethoxy)-N,N-bis(2-picolyl) amine and MnCl2 into aqueous solution in a molar ratio of 1 to 1, and controlling the temperature to be between 20 and 40 DEG C; and synthesizing ammonium chloride and a catalyst in a molar ratio of the ammonium chloride to the MnCl2 of 0.2 to 1, reacting the mixture at the temperature of 30 DEG C for 1 to 4 hours, purifying a product by using silica gel column chromatography, concentrating the product and removing the solution to obtain light yellow manganese compound. The manganese compound is applied in the aspect of magnetic resonance imaging in a liver cancer body; and compared with the blank aqueous solution without the manganese compound, the compound can remarkably improve the tumor diagnosis effect, has magnetic resonance imaging function and tumor targeting property, and can be used as a magnetic resonance imaging contrast agent for the tumor.

A novel substituted N-acetyl-L-cysteine (NAC) derivative and methods of using this compound for the treatment of diseases and/or conditions, including but not limited to diseases and/or conditions of, or involving, the Central Nervous System (CNS), including schizophrenia adrenoleukodystrophy, mitochondrial diseases (e.g. Leigh syndrome, Alpers' disease, and MELAS), Huntington's disease, trichotillomania, HIV-associated neurocognitive disorder, hypoxic-ischemic encephalopathy, drug craving, and drug addiction.

The invention discloses a method for preparation of propionic acid with alcohol by carbonylation. The pretreating technique to active carbon is: treating with deionized water, drying, treating with non- organic acid and cleaning with deionized water to make it neutral, and drying. The catalyst which is supported by metallic salt solution several times is burnt in 400- 600Deg. C high temperature and in a condition of reducing gas in order to be used in the reaction process. Dissolving part soluble material in the active carbon, and none destroying the bone structure of the active carbon, it improves specific surface area and absorption ability of the active carbon, and improves the conversion rate of alcohol and the total yield of propanoic and acid propionic ether.

The invention discloses a production technology for synthesis of ethyl 2-bromopropionate and relates to the technical field of chemical engineering. The 2-bromopropionyl chloride is prepared by steps of carrying out the acylating chlorination reaction for sulfoxide chloride, propionic acid, red phosphorus and dry bromine, and then carrying out esterification reaction between the 2-bromopropionyl chloride serving as a raw material and anhydrous ethanol to obtain the ethyl 2-bromopropionate, filtering and distilling. The production technology disclosed by the invention has the beneficial effects that the preparation is convenient and easy, and environment-friendly without pollution, the raw materials are easily available, the equipment investment is small, the purity is high, the operation is convenient, and the prepared ethyl 2-bromopropionate is good in using effect, safe and reliable.

The invention relates to a synthesizing process of 2,3-dicyanoethylpropionate. The process comprises the steps that: electric stirring is started; dimethyl sulfoxide is sucked by using vacuum, and a cooling valve is opened for cooling; ethyl cyanoacetate is sucked; when the temperature is reduced to 4-6 DEG C, paraformaldehyde is added, and sodium cyanide is added; when dosing is finished; heating is carried out for azeotropy; sodium thiosulfate is added, and hydrochloric acid is dropped in, such that a pH value reaches 3-4; a dichloroethane extractant is rapidly added, and the mixture is settled and stratified; an upper-layer material and dichloroethane are delivered to a secondary reaction kettle, and lower-layer water and dimethyl sulfoxide are recovered; the stratified material is pumped into a desolventizing kettle, and dichloroethane is recovered, such that a 2,3-dicyanoethylpropionate crude product is obtained; and rectification is carried out, such that a 2,3-dicyanoethylpropionate finished product is obtained. The process provided by the invention has the advantages that: the synthesizing temperature is controlled at 5+/-1DEG C; reaction is smooth; side reaction is prevented; and yield is high. The extraction effect of dichloroethane upon the 2,3-dicyanoethylpropionate crude product is better, wherein an extraction rate reaches 97%, such that product yield is greatly improved.

The invention discloses a preparation method of an anti-hepatitis C medicine sofosbuvir. The method comprises the following steps: taking r-ethyl glycerate acetonide as an initial raw material, enabling the r-ethyl glycerate acetonide to react with ethyl alpha-fluoropropionate under the action of potassium tert-butoxide, performing carbonyl reduction, hydroxyl acylation, hydrolytic cyclization under an acidic condition, hydroxyl acylation, red aluminum reduction and chiral column separation so as to obtain a sofosbuvir key intermediate ((2R,3R,4R,5R)-3-(benzoyloxy)-5-hydroxy-4-fluoro-4-methyltetrahydrofuran-2-yl) methyl benzoate, performing 2-hydroxyl acetylation, enabling acetylized material to react with 2-trimethylsiloxy-4-benzamidopyrimidine, removing benzamido under an acidic condition, performing dehydroxylation protection, and finally enabling obtained material to react with N-[(S)-(2,3,4,5,6-Pentafluorophenoxy)phenoxyphosphinyl]-L-alanine 1-methylethyl ester to obtain the sofosbuvir. The method has the advantages of short synthesis route, high yield, avoidance of a fluorination reaction step in the synthesis process, and mild synthesis reaction conditions.

The invention discloses a preparation method of a 3-(2-pyridineamino)ethyl propionate. The method comprises the following steps: performing catalytic reaction by using 2-aminopyridine and ethyl acrylate as a raw material, and using a Bronsted acid loaded by silicagel as a catalyst in an inorganic solvent or an organic solvent and controlling temperature at 80-120 DEG C through oil bath heating, wherein the temperature of the obtained reaction mothersolution is 40-45 DEG.C, concentrating at the pressure of 0.09-0.1MPa at reduced pressure, performing the chromatography on the concentrated solution through a silicagel column or an aluminum oxide column to obtain 3-(2-pyridineamino)ethyl propionate. The preparation method of the 3-(2-pyridineamino)ethyl propionate has the characteristics of simple preparation method, convenience in operation, low production cost, and short reaction time; the used silicagel-loaded Bronsted acid catalyst can be recycled, and the product yield of the finally obtained 3-(2-pyridineamino)ethyl propionate achieves 50-76%.

The invention discloses a method for preparing propionic acid from ethyl acetate through carbonylation. A reaction system consists of ethyl acetate, a main catalyst, a co-catalyst and water according to a molar ratio of 1:0.01-0.0001:0.05-0.5:1-10, wherein the reaction temperature is 140-300 DEG C, and the carbon monoxide pressure is 2.0-10.0 MPa; the main catalyst is a rhodium compound; the co-catalyst is iodoethane; an iodide additive such as hydriodic acid, lithium iodide, potassium iodide, tin iodide, lead iodide, zinc iodide or cadmium iodide, a polar solvent such as acetic acid, propionic acid or butyric acid and an organic ligand are selectively added into the reaction system; the molar ratio of the iodide additive to the ethyl acetate is 0.01-1; the molar ratio of the polar solvent to the ethyl acetate is 0.1-10; and the molar ratio of the organic ligand to the main catalyst is 1-5. The process raw materials are freely and economically selected, the problem that ethanol is hydrolyzed and esterified to produce diethyl ether and propionic acid under an acidic condition is solved, and the selectivity of the propionic acid is improved.

The invention relates to the technical field of organic synthesis and bulk drug intermediates, and concretely relates to a preparation method of a key intermediate 4-hydroxyquinoline-3-carboxylic acid of a new medicine ivacaftor for treating cystic fibrosis. The preparation method comprises the following steps: 1, carrying out a condensation reaction: reacting o-nitrobenzoic acid, potassium monoethyl malonate and N,N-carbonyldiimidazole to prepare ethyl 3-(2-nitrophenyl)-3-oxopropanoate; 2, carrying out a reduction reaction: carrying out catalytic hydrogenation reduction on ethyl 3-(2-nitrophenyl)-3-oxopropanoate to prepare ethyl 3-(2-aminophenyl)-3-oxopropanoate; 3, carrying out a cyclization reaction: carrying out nucleophilic addition and cyclization reaction on ethyl 3-(2-aminophenyl)-3-oxopropanoate and N,N-dimethyl formamide dimethyl acctel to obtain ethyl 4-hydroxyquinoline-3-carboxylate; and 4, carrying out a hydrolysis reaction: carrying out the hydrolysis reaction on ethyl 4-hydroxyquinoline-3-carboxylate to obtain 4-hydroxyquinoline-3-carboxylic acid. The preparation method has the advantages of easily available raw materials, mild reaction conditions, simplicity and convenience in post-treatment, suitableness for amplified preparation, and high yield.

The invention relates to a method for preparing ethyl acetylpropionate by catalyzing furfural via a one-pot method, and relates to ethyl acetylpropionate. The method comprises the following steps of heating furfural, a catalyst and ethyl alcohol in a reaction kettle, cooling to room temperature, centrifuging and decomposing, obtaining a liquid phase, and purifying, so as to obtain ethyl acetylpropionate; using the solid as the recycling catalyst. The method has the advantages that furfural is directly used as the raw material to prepare ethyl acetylpropionate; used ethyl alcohol can be simultaneously used as reaction raw material, solvent and hydrogen donor, the external hydrogen source and other solvents are not needed, and the reaction system is simple, so as to conveniently separate thetarget product and recycle and reutilize the solvent; the preparation procedure of a dual-function molecular sieve-loaded catalyst for simultaneously catalyzing the transfer hydrogenation and alcoholysis reaction is simple, the price of the raw material is low, and ethyl acetylpropionate with higher yield rate can be obtained by catalyzing furfural; the used catalyst can be conveniently recycled,and the activity is still stable after recycling.