1405 results about "De esterification" patented technology

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 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 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 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 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 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 relates to fields of daily chemicals and pharmaceuticals industry, in particular to 6-amino-6-deoxyinulin as well as preparation and application thereof. In the 6-amino-6-deoxyinulin shown as a formula (I), the average value range of n is 10-35. The preparation comprises the steps of undergoing a helogenation reaction of inulin or undergoing esterification of inulin and sulfonyl chloride, respectively undergoing a reaction of the product obtained through the helogenation reaction of the inulin or the esterification and sodium azide or azido lithium at a temperature of 40-70 DEG C for 8-24 hours to obtain 6-azido-6-deoxyinulin, and reducing the 6-azido-6-deoxyinulin by utilizing triphenylphosphine or lithium aluminium hydride to obtain the 6-amino-6-deoxyinulin. In the invention, the 6-amino-6-deoxyinulin is obtained through an effective synthetic means; an inulin six-position easily-leaving group is obtained through utilizing halogen to substitute the primary hydroxyl ofthe inulin or through the esterification of inulin and sulfonyl chloride; and the 6-amino-6-deoxyinulin with high substitution is obtained through azido nucleophilic substitution and reduction. The 6-amino-6-deoxyinulin synthesized by the preparation method provided by the invention is simple in the synthetic step and easy to popularize; and the required equipment and raw materials are easy to get. The formula (I) is shown in the specification.