1418 results about "De esterification" patented technology

The use of an N,N-dimethyl alkylamide or an N-alkanoyl morpholine provides a stable emulsifiable concentrate composition that hinders de-esterification and transesterification of mixtures of a carboxylic acid herbicide and an ester of a different carboxylic acid herbicide. The N,N-dimethyl alkylamide or N-alkanoyl morpholine additionally stabilizes emulsifiable concentrates containing a triazolopyrimidine herbicide having at least one methoxy group on the triazolopyrimidine ring.

[Aim]This invention relates to a makeup containing a specific modified silicone obtained by an economical manufacturing method not requiring an esterification catalyst, having a high reaction rate and therefore leaving little unreacted material, and in particular relates to a makeup with good skin adhesion, good retention and excellent emulsion stability. [Composition]A silicone compound represented by the general formula (1): <paragraph lvl="0"><in-line-formula>R1aR2bSiO (4-a-b) / 2 < / in-line-formula>(in the formula, R1 is at least one substituent group having 1-30 carbon atoms, chosen from alkyaryl, aralkyl, fluorine-substituted alkyl or organopolysiloxanylsilyl, R2 is a carboxylate residue represented by the following general formula (2): R3is a saturated or unsaturated hydrocarbon group having 2-30 carbon atoms, a is 1.0-2.5, and b is 0.001-1.5.

The invention discloses a making method of C1-C4 alkyl ester of nitrous acid, which comprises the following steps: doing the oxidizing reaction and esterifying reaction in two reactors separately; doing the oxidizing reaction in the oxidizing reactor; doing the esterifying reaction in the esterifying tower reactor; inputting nitrogen oxide, oxygen and one or more of inert gas into oxidizing reactor; selecting the nitrogen oxide from one or more composite gas of NO, N2O3, NO2 and N2O4 with NO constantly; making the mole of NO more than the mole of NO2; using 0.15-0.3 m oxygen for each NO m; making the bulk of inert gas at 0-90% corresponding to total gas; inputting the oxidizing reacting product into the esterifying tower reactor to react with C1-C4 alkanol; using 0.8-3.0 m alkanol for each gram atom nitrogen. The invention can transfer heat effectively to reduce by-product, which is smaller than traditional equipment.

The invention relates to quercetin-3-O-acyl ester and a preparation method thereof and belongs to the technical field of pharmaceutical chemistry. The preparation method comprises the following steps: taking cheap rutin as a starting raw material and preparing a quercetin-3-O-acyl ester compound through benzylation, hydrolysis under the acidic conditions, esterification, catalytic hydrogenolysis and other reactions. The method has the characteristics of good selectivity, mild reaction condition, high yield, low cost, simplicity and convenience in operation, easiness in industrial production and the like. In addition, the inhibitory effect of the obtained quercetin-3-O-acyl ester on human esophageal squamous carcinoma cells EC9706, human prostatic cancer cells PC-3 and human gastric cancer cells MGC-803 is remarkably superior to that of quercetin; and the quercetin-3-O-acyl ester can be used in the field of foods and medicines and is possible to develop into a new candidate drug for treating tumor.

Diols produced in fermentation are processed in broth by esterification of the product diol with a carboxylic acid (e.g., fatty acid) and a catalyst (e.g., lipase) capable of esterifying the product diol, such as 1,3-propanediol, with the carboxylic acid to form the diol esters. The diol esters can be extracted from the broth, and the product diol recovered from the diol esters. The carboxylic acid can also serve as an extractant for removal of the diol esters from the fermentation medium.

This invention discloses a new camptothecin derivate of 20-position esterification, its preparation, containing their medicine combination, and its usage of using it as medicine, especially as antitumor drug.

The invention relates to 1,3-propanediol and a preparation method thereof. Firstly, through the melt esterification reaction between dibasic acid and pentaerythritol, DAPER with the terminal group being carboxyl is prepared; then, DADA with the terminal group containing carboxyl is prepared through the melt condensation reaction between the double-functional-group organic acid containing functional elements and dihydric alcohol; the double functional groups in the double-functional-group organic acid containing functional elements are selected from phosphate, carboxylic group and hydrosulphonyl; the functional elements are one kind of materials from P, S and N, or the combination of S and N; finally, the DAPER is added into the DADA to prepare the final product through the esterification reaction between the DAPER and the DADA. The defects of storage and use difficulty, single purpose due to simple structure, environment pollution in the preparation process and the like of the conventional liquid type 1,3-propanediol are overcome. The finally prepared 1,3-propanediol is solid materials with the high molecular weight; the terminal group of the molecule is a reaction active group; 8.14 to 18.32 weight percent of functional elements are contained inside the terminal group of the molecule; the advantages of high thermal stability, wide purposes and the like are realized.

The invention discloses a method for synthesizing and purifying high-purity fatty acyl monoglyceride, which comprises the following steps: (1) mixing fat, free fatty acid and a solid catalyst, vacuumizing, stirring, heating, obtaining a mixture of fat, adding glycerol into the mixture of fat, performing refluxing esterification and ester exchange reactions, controlling the temperature of cooling water in a reflux condenser to allow water generated in esterification to be pumped out under vacuum and allow glycerol to be condensed and refluxed, and demixing the products of the reaction, wherein the upper layer is a glyceride layer; (2) removing unreacted free fatty acid and glycerol from the glyceride layer through primary molecular distillation; and (3) subjecting the glyceride layer from which the free fatty acid and glycerol are removed to secondary molecular distillation, and obtaining a distillate and a distillation residue, wherein the distillate is high-purity fatty acyl monoglyceride and the distillation residue is diglyceride or triglyceride. When the method is used, the process is shortened, equipment investment is saved, and the primary yield of the product is increased greatly.

The invention provides a method utilizing high acid value oil as raw material for preparing biodiesel. Various animal and vegetable oil, the acid value of which is larger than 3.0mg KOH / g oil, oilstock, soapstock and acidic oil in a vegetable oil refining process, various food waste oil (restaurant waste oil, hogwash oil, trench waste oil, and the like) and various waste animal oil in industrial processing (waste animal oil in leather processing, waste animal oil in slaughtering process, and the like) are used as raw materials to obtain biodiesel products by filtration for removing solid impurities, vacuum dehydration, stratified graded acid catalytic esterification, alkali catalytic transesterification and vacuum distillation. The method utilizing the high acid value oil as the raw material for preparing the biodiesel has the beneficial effect that the production process can be applied to raw materials with different acid values to produce biodiesel products with high purity by changing the operational series of the stratified graded acid catalytic esterification reaction and has the advantages of simple process, low energy consumption, high conversion rate and small device. And continuous production can be realized.

The invention relates to a manufacturing method of atorvastatin intermediate (R)-(-)-4-nitrile-3-hydroxybutyrate (ATS-5), which solves the problems of high cost, expensive raw material price and the like of the prior art. The manufacturing method is characterized in that the atorvastatin intermediate is prepared from epichlorohydrin as a raw material through ring-opening addition, glycolysis esterification, cyaniding substitution synthesis and refining. The invention has simple synthesis route, abundant raw material resources, low equipment requirements and no high-temperature high-pressure reaction; the content of produced ATS-5 is more than 98 percent, the content of water is lower than 0.2 percent, and the content of enantiomer is less than 1.0 percent. The manufacturing method is a mature production process for manufacturing the intermediate of medicine atorvastatin and is applicable to medium-sized and small enterprises.

The invention relates to a synthetic method of 2-methallyl alcohol. The synthetic method comprises the step of carrying out esterification reaction, refinement and separation and hydrolysis reaction on 2-methallyl chloride and sodium carboxylate to prepare 2-methallyl alcohol, wherein the formulas of the esterification reaction and the hydrolysis reaction are respectively formula (1) and formula (2) both referring to the description; the R is CH3 or CH3CH2, namely, methyl or ethyl. According to the invention, the synthetic method is reasonable in technology and easy to operate; the product is high selectivity and relatively high in quality; carboxylic sodium in the esterification reaction stage and water in the hydrolysis reaction stage are recycled and need no external supplement, so that cyclic utilization is achieved, and the product yield is improved.

The invention relates to a continuous production process for DOP (Dioctyl Phthalate) and used equipment, which belong to the technical field of fine chemical production. The continuous production process comprises the following steps of: firstly carrying out esterification reaction of phthalic anhydride and isooctyl alcohol in the presence of a catalyst such as titanate, and then carrying out dealcoholization, neutralization and water washing, steam stripping and drying, adsorption and filtration to obtain the DOP. In the invention, by adopting six esterification kettles which are connected in series and have completely the same structure for the esterification reaction, alcohol is kept excessive, the conversion rate is high and is larger than 99.5 percent, the acid value of coarse ester generated in the reaction is less than or equal to 0.3mgKOH / g, and the excessive alcohol accounts for 16 percent; by using the equipment, a production method with low energy consumption, high production capacity and continuous esterification is obtained, the conversion rate is high, the production quantity of a device is improved, the production cost is lowered, and the continuous production process is suitable for industrialized production; the excessive alcohol and the water generated in an esterification stage are recycled and comprehensively recovered, so that the generation of three wastes is reduced; and the production capacity of the DOP is enlarged by 50 percent as compared with a single set of domestic device, and the consumption of energy sources is decreased by 20 percent.

The present invention relates to a marine organism anti-fouling paint and a preparing method and use thereof. The marine organism anti-fouling paint is polyacrylic-capsaicin resin, and the preparing method thereof comprises the steps of: performing esterification reaction for capsaicin compounds and acrylic acid or acrylic acid derivatives to obtain polyacrylic-capsaicin esters; and performing polymerization for the polyacrylic-capsaicin esters and acrylic ester compounds to obtain the polyacrylic-capsaicin resin. The method of the present invention directly performs chemical synthesis for natural organic-compounds with the functions of antimicrobial, sterilization and marine organism repelling action and the anti-fouling paint ground mass, then coats the prepared polyacrylic-capsaicin resin and the anti-fouling paint ground mass onto a body of a ship, after that, in the environment of seawater, the capsaicin in the resin can release slowly to restrain adhesion of the marine organism, thus the anti-fouling paint has the advantages of long aging, nontoxicity, green and environment protection, can be widely applied to prevention and cure for organism fouling, and has wide application prospects and economic values.

The invention relates to application of lipase SMG1 in preparation of fatty acid monoglyceride, which comprises the following steps of: (1) preparing glycerol and fatty acid donor, adopting partial glyceride hydrolase SMG1 from Malasseziaglobosa as catalyst, and adding 1%-5% of water to catalyze reaction of the glycerol and fatty acid donor at 5-15 DEG C; and (2) separating, and removing lipase and glycerol from the product obtained from the step (1), separating and removing diglyceride and fatty acid to obtain the fatty acid monoglyceride. The glycerol and fatty acid donor can be used as a raw material in the invention, and esterification of the glycerol and fatty acid donor is catalyzed through lipase SMG1 at low temperature so as to generate the fatty acid monoglyceride. The prepared product has few by-products, light color and high yield.

The invention relates to a method for continuous enzymatic synthesis of n-3PUFA glyceride, comprising the following steps: preparing fish oil n-3PUFA (EPA, DHA) and glycerol into reaction liquid according to a certain proportion; then pumping reaction liquid into an enzyme reaction column provided with immobilized lipase through a constant current pump for carrying out reaction for enzymatic synthesis of n-3PUFA; finally realizing continuous enzymatic synthetic production of n-3PUFA by controlling circulation flow velocity of the reaction liquid in the reactor and setting a molecular sieve dehydrater in the reaction system. The n-3PUFA glyceride product prepared by the continuous syhthesis method features an ester yield of 30-50%, a monoester content of 20-30%, a diester content of 50-70%and a trig content of 10-20%. With the method of the invention adopted, recycle of enzyme can be realized, cost can be greatly reduced, production cycle can be shortened, production efficiency can beimproved and the operation is easy, so that the method is of great practical value to industrialized batch production.

The invention relates to a new synthesis technology of anti-cancer drug Raltitrexed. The technology comprises the following steps: 1) using L-glutamic acid as raw material to perform esterification with alcohol under the action of halogenating agent and obtain L-glutamic acid diester hydrochloride; 2) using 2-amino-5-methyl-benzoic acid as raw material to prepare 6-bromomethyl-3,4-dihydro-2-methyl-4-oxo-6-quinazoline through cyclization, amination and bromination; 3) using 2-thienyl-propanedioic acid as raw material to prepare N-[5-[N-(tert-butoxycarbonyl)-N-methylamino]-2-thenoyl]-L-glutamic acid diethyl ester through nitrification, esterification, reduction, amino protection, N-methylation and device-esterification; 4) using L-glutamic acid diester hydrochloride and N-[5-[N-(tert-butoxycarbonyl)-N-methylamino]-2-thenoyl]-L-glutamic acid diethyl ester to prepare N-[5-(N-methylamino)-2-thenoyl]-L-glutamic acid diester through dehydrant condensation and deamination protection; and 5) using N-[5-(N-methylamino)-2-thenoyl]-L-glutamic acid diester and 6-bromomethyl-3,4-dihydro-2-methyl-4-oxo-6-quinazoline to perform condensation under the catalysis of alkali, recycling preparative chromatography, purifying, and performing de-esterification to obtain Raltitrexed.

The invention discloses a method for deacidifying and refining high-acid value fish oil by using an enzyme method, comprising the following steps of: firstly, selectively esterifying free fatty acid reacting with alcohol in the fish oil by adopting immobilized lipase as a catalyst, and then neutralizing to obtain the refined fish oil. Compared with the traditional chemical refining method, because the method greatly reduces the acid value of grease, the refining yield is greatly improved, and the method has better economical efficiency and environmental protection feature.

The invention relates to the utilisation of fatty acid feedstockin the production of biodiesel by the use of microbial enzymes.

The invention provides a stilbene derivative with 1,3,4-oxadiazole and a preparation method and application thereof. The preparation method of the stilbene derivative with 1,3,4-oxadiazole comprises four specific reaction steps, namely oxidation cyclization reaction, NBS (N-bromosuccinimide) bromination reaction, triethyl phosphite esterification reaction and Wittig-Honner reaction. The stilbene derivative with 1,3,4-oxadiazole disclosed by the invention can be used to obviously inhibit the growing activities of Lepidopteron such as beet armyworm and cabbage looper and have important application value in the developments of environmentally friendly, efficient and new pesticides.

The invention discloses a preparation method for tedizolid as shown in a formula IV. According to the method, tedizolid is prepared through chemical combination of a compound as shown in a formula I and a compound as shown in a formula II via a coupling reaction; and tedizolid phosphate with medical purposes can be prepared by subjecting the obtained tedizolid to esterification by phosphate. The preparation method has the advantages of milder reaction conditions, a few produced impurities and simple post-treatment. According to the invention, the reaction mechanism of Suzuki-Miyaura coupling is employed to connect boric acid as shown in the formula I and derivatives thereof with the compound as shown in the formula II, so reaction selectivity is high, a few impurities are produced, and a synthetic ratio is more than 90%; and oxazolidinone borate is used to react with tetrazole, so conditions are milder, and the generation rate of impurities is lower.

The invention discloses a method for synthesizing a polylactic acid-block-polyN-isopropyl acrylamide temperature-sensitive material, and belongs to the technical field of amphipathy block copolymers. The method comprises the following steps of: initiating ring-opening polymerization of L-lactide by using tetra(2-hydroxyethyl) phenyl porphyrin to prepare hydroxylated star-shaped polylactic acid taking porphyrin as a core terminal; carrying out esterification reaction on the hydroxylated star-shaped polylactic acid taking porphyrin as the core terminal to obtain a macromolecular chain transfer agent; and preparing a novel star-shaped polylactic acid-block-polyN-isopropyl acrylamide temperature-sensitive material from the macromolecular chain transfer agent and a temperature-sensitive N-isopropyl acrylamide monomer by using a reversible addition-fragmentation chain transfer polymerization method. According to the method, a mild polymerization condition is adopted to facilitate the preparation of the star-shaped polylactic acid-block-polyN-isopropyl acrylamide temperature-sensitive biological material with polyN-isopropyl acrylamide adjustable in length and porphyrin as a core.

The invention belongs to the technical field of new drug synthesis, and in particular relates to an IDO inhibitor containing (E)-4-(beta-bromovinyl)phenoxy acyl structure, as well as a preparation method thereof. The preparation method comprises the following steps: solvent benzene, (E)-4-(beta-bromovinyl) phenol, carboxylic acid and p-dimethylaminopyridine are added to a flask respectively and magnetically stirred for 5 to 20 minutes at room temperature; then N, N'-dicyclohexylcarbodiimide is added and reacts for 2 to 24 hours at room temperature; after the reaction is completed, the solvent benzene is steamed off after decompression; residue is subjected to column chromatography separation and purification by taking ethyl acetate / petroleum ether as leacheate, and then a needed product can be obtained, wherein the molar ratio of the solvent benzene to the (E)-4-(beta-bromovinyl) phenol is 50-200:1; the molar ratio of the carboxylic acid to the (E)-4-(beta-bromovinyl) phenol is 1-1.5:1; the molar ratio of the p-dimethylaminopyridine to the (E)-4-(beta-bromovinyl) phenol is 0.1-1.5:1; and the molar ratio of the N, N'-dicyclohexylcarbodiimide to the (E)-4-(beta-bromovinyl) phenol is 1-1.2:1. The method takes the (E)-4-(beta-bromovinyl) phenol as a synthesis building block and obtains a series of the novel IDO inhibitors containing the (E)-4-(beta-bromovinyl)phenoxy acyl structure through esterification reaction, and the IDO inhibitors can be used for treating the diseases with the pathological features of IDO mediated tryptophan metabolic pathway.

The invention relates to a method for preparing microcrystalline cellulose by using carrot pomace, belonging to the technical field of edible materials. The preparation method comprises the following steps: 1. pretreatment; 2. treatment with hydrochloric acid; 3. sodium hydroxide treatment with sodium hydroxide; 4. de-esterification with alcohol; 5. bleaching with sodium hypochlorite; and 6. hydrolysis with hydrochloric acid. The microcrystalline cellulose prepared by the carrot pomace obtained in the invention can be widely used for medicine, food and daily chemical industries, and the preparation process is simple and easy to implement and is low in cost; the carrot pomace is used as a raw material, thereby not only increasing added values of deep processing of carrots, reducing the production cost of the microcrystalline cellulose, enriching the source of raw materials for producing edible fibers, but also being favorable for reducing environmental pollution.

The invention provides a method for simultaneous detection of 3-chloropropanol ester and glycidyl ester in food. The method comprises the following steps: 1) pretreatment of a sample: dividing a food sample into two equal parts which are respectively used as food samples for a sample testing group A and a sample testing group B, and separately adding an internal standard solution into the food samples for ultrasonic extraction; 2) an ester interchange reaction: subjecting to-be-reacted solutions of the sample testing groups A and B to a hydrolysis reaction, then respectively adding a sodium chloride-acetic acid solution and a sodium sulfate-acetic acid solution into the reaction systems of the sample testing groups A and B to terminate the hydrolysis reaction, and then separately carrying out de-esterification with n-hexane; 3) a derivative reaction: adding a phenylboronic acid solution into residues obtained after de-esterification of the sample testing groups A and B for the derivative reaction;and 4) GC-MS detection and analysis. The method provided by the invention can simultaneously detect 3-chloropropanol ester and glycidyl ester in food, has high detection efficiency and is applicable to detection of a plurality of food samples.

The invention provides a preparation method of sucrose 6 ester. The preparation method comprises the following steps: preparing a reaction solution of sucrose and an organic tin compound; atomizing the reaction solution to form small liquid drops; fully mixing and contacting the droplets with a gasified dehydration medium, and carrying out dehydration reaction on the droplets so as to generate anintermediate mixture containing the sucrose organic tin ester droplets; separating the intermediate mixture to obtain a sucrose organic tin ester solution and a dehydrated gas-liquid mixture; recovering the sucrose organic tin ester solution obtained in the separation step and circulating the sucrose organic tin ester solution to the atomization step and the dehydration step for multiple times; and carrying out acylation reaction on the sucrose organic tin ester solution and organic anhydride to generate sucrose 6 ester. According to the method, rapid and efficient dehydration of the esterification reaction can be realized in an extremely short time, the sucrose organic tin ester intermediate is efficiently prepared, decomposition of carbohydrates and side reactions in the system are reduced to a great extent, the energy consumption is low, the product yield is high, the selectivity is high, and the sucrose reaction degree is more thorough.

The present invention is directed to improving productivity of an enzymatic method for producing esterified, transesterified or interesterified fats or oils. Specifically, a method that can greatly improve the productivity of enzymatic esterification, transesterification or interesterification by purifying the substrate oil to extend the useful life of the enzyme is disclosed.

The invention discloses two synthetic methods of a diamondback moth sex pheromone compound. The first method adopts 1,11-undecadiol and n-amyl bromide as initial raw materials, and comprises four-step reactions including a critical Wittig reaction to synthesize (Z)-11-hexadecen-1-yl acetate, a hydrolytic reaction to obtain (Z)-11-hexadecen-1-ol, and a pyridinium chlorochromate oxidation reaction to obtain (Z)-11-hexadecenal. The second method adopts 1,11-undecadiol and valeraldehyde as initial raw materials, and comprises three-step reactions including a critical Wittig reaction to synthesize (Z)-11-hexadecen-1-ol, a pyridinium chlorochromate oxidation reaction to obtain (Z)-11-hexadecenal, and an esterification reaction to obtain (Z)-11-hexadecen-1-yl acetate. The invention has the advantages of cheap and easily available raw materials, simple synthetic route, mild reaction condition, convenient and safe operation, high yield, and low cost.

The present invention discloses a preparation method of slowly-digestible starch-based recombinant rice with a low glycemic index, and belongs to the technical field of food processing. After a high-temperature fluidization technology is used to conduct a non-crystallizing treatment of a solid-phase broken rice raw material in a short time, materials are subjected to a one-step reactive extrusiontechnology, enzyme-adding enzymatic hydrolysis and an esterification treatment are combined, and the recombinant rice with high slowly-digestible starch content and low glycemic index is obtained. Therecombinant rice prepared by the one-step shaping extrusion technology is suitable for consumption of patients with type II diabetes. At the same time, the preparation method increases added value ofagricultural and sideline products, reduces production cost, and improves production efficiency.

The invention discloses a method for preparing cetilistat, which belongs to the technical field of the medicine preparation method, and is used for solving the problems of high three wastes, low yield and high cost in the current preparation method. The method comprises the following steps: 1)esterifying a compound A(2-amino-5-methyl benzoic acid) or its salt; 2) acylating an esterification object in the step 1) and chloroformic acid n-cetanol ester; 3)removing ester group of the compound obtained in the step 2) to obtain 2-(cetane carbonyl oxygen)amino-5-methyl benzoic acid; and 4)cyclizing the compound in the step 3) to obtain the target products. By improving the production steps, the invention provides the synthetic method with simple operation, high efficiency, and convenient industrial production for the cetilistat product.

The invention relates to the technical field of a reserving agent for washing, particular to the reserving agent for washing jean garments and a preparation method thereof. The reserving agent is generated by carrying out esterification reaction on polyether dicarboxylic acid and ethylene glycol serving as raw materials under the action of an acid catalyst, wherein the molar ratio of the polyether dicarboxylic acid and the ethylene glycol is 1:1; and the reserving agent is water-solubility macromolecule polyester. The reserving agent provided by the invention is a non-ionic surface active agent and is not combined with protein in the washing and fade-out treatment process of the jean garments, and therefore, the catalytic activity of the reserving agent can be remained, and the reserving effect has excellent back-staining resistant effect. The preparation method provided by the invention is simple in production process, is convenient for realizing large-scale production and has good production prospect and market application prospect.