40 results about "N acylation" patented technology

The invention discloses a preparation method of high-purity cefuroxime acid which is an intermediate for synthesizing second-generation cephalosporins cefuroxime sodium and cefuroxime axetil. The preparation method comprises the following steps: based on 7-aminocephalosporanic acid (7-ACA) as a raw material, carrying out an N-acylation reaction on the 7-ACA and furoyl acetylcholine at the 7-position; at a low temperature, hydrolyzing 3-acetyl with a sodium hydroxide solution, crystallizing, filtering and drying so as to obtain the intermediate 3-deformamido cefuroxime acid (DCC); quantitatively adding the DCC in a tetrahydrofuran solvent, dropwise adding chlorosulfonyl isocyanate for a nucleophilic addition reaction so as to generate chlorosulfonyl cefuroxime acid, and adding purified water for hydrolysis so as to prepare a cefuroxime acid reaction liquid; adding sodium bicarbonate for salifying; removing by-reactant lactone and other unsaponifiable impurities in the reaction liquid with a ternary compound extracting agent of dichloromethane, ethyl acetate and tetrahydrofuran, layering, and adding hydrochloric acid in a water phase for acidification; adding the ternary compound extracting agent to extract and separate out the cefuroxime acid; and removing water-soluble impurities, crystallizing and filtering a distilled organic phase, and then drying so as to obtain the high-purity cefuroxime acid with the purity of more than or equal to 99%.

The present invention provides a method for the N-demethylation and/or N-acylation of an N-methylated heterocycle such as morphine alkaloids or tropane alkaloids. The method comprises reacting the heterocycle with an acylating agent in the presence of a metal catalyst.

The invention belongs to the field of chemical synthesis, and particularly relates to a synthetic method of a ceftriaxone sodium crude salt. The method comprises the following steps of: (1) performing electrophilic substitution on 7-ACA and a triazine ring by taking a BF3-acetonitrile solution as a catalyst to obtain 7-ACT at last; and (2) undergoing an N-acylation reaction on 7-ACT and AE-active ester in an organic phase, adding sodium iso-octoate, and undergoing a salt forming reaction to obtain the ceftriaxone sodium crude salt. The method is characterized in that: the 7-ACT is prepared with an enzymatic hydrolysis method after electrophilic substitution in the step (1); and a flocculating agent is added after the N-acylation reaction is completed in the step (2). The method has the advantages that: the product yield and purity are raised; the 7-ACT is prepared with the enzymatic hydrolysis method in the first step, and the enzymatic hydrolysis method has the characteristics of specificity and high efficiency, so that side reactions are avoided, the yield is increased by over 8 percent, and can be up to 88 percent, and the product purity is raised; and the flocculating agent is added in the second step, so that insoluble matters in a reaction liquid are removed, and a high-purity ceftriaxone sodium crude salt is obtained finally.

The invention discloses a preparation technology and a refining method of ranolazine, which are more suitable for industrial production. The method comprises the following concrete steps: using 2, 6-dimethylaniline and methylpyrocatechine as original materials; sequentially carrying out four reaction processes of N-acylation, O-alkylation, N-alkylation and N-alkylation to synthesize ranolazine; and then, recrystallizing to obtain a refined product. The refined product obtained by the method has high purity, and the method also has the advantages of simple operation, low production cost and high yield and is more suitable for industrial production.

The invention discloses a one-pot synthesis method of an N-hydrocarbon acyl cyclic lactam derivative. The method comprises the following steps: adding lactam and acyl chloride into a reaction kettle, stirring, performing N-acylation reaction, slowly adding a weak alkali compound into the reaction kettle to neutralize acid generated in the N-acylation reaction, reacting for a while, further adding hydroxylamine and a weak alkali compound or only adding the weak alkali compound into the reaction kettle, and performing open loop reaction to obtain a N-hydrocarbon acylamino hydroximic acid salt or N-hydrocarbon acylamino carboxylate. The method adopts a one-pot synthesis method, is gentle in reaction condition, high in yield, low in cost, easy to operate and short in production period, and the industrial production is met.

The invention discloses a method utilizing a micro-reactor to continuously synthesize amide herbicide, and belongs to the technical field of organic synthesis. The method takes substituted aniline as the raw material, and then the substituted aniline is subjected to continuous two steps of N-acylation and heterogeneous N-alkylation in a micro-reactor so as to obtain the amide herbicide; wherein the conversion rate of substituted aniline can reach 98% or more, the total yield of the reactions can exceed 95%, and the product purity is more than 96%. The intermediate purifying step is saved, thus the production procedure is simplified, the reaction time is reduced, the alkali solution consumption is reduced, the production equipment is simple, the production efficiency is high, and the product yield and purity are high.

The present invention provides a method for analyzing the C-terminal amino acid sequence of a peptide by using a reaction for successively releasing the C-terminal amino acids of the peptide, which method can suppress, when successively releasing the C-terminal amino acids of a peptide of long amino acid length, such a undesirable side reaction as cleavage of peptide bond in the intermediate position of the peptide and can carry out the chemical treatment thereof under widely applicable conditions; In the method, a dry sample of a peptide with long amino acid length is beforehand subjected to an N-acylation treatment; by using a reaction reagent where an alkanoic acid anhydride is combined with a small amount of a perfluoroalkanoic acid, successive release of C-terminal amino acids is conducted under mild conditions; a hydrolysis treatment is applied; then, selective fragmentization at site of arginine residue is performed by digestion by trypsin; thereafter, decreases in molecular weight are measured for the C-terminal side fragments derived from a series of reaction products with use of a MALDI-TOF-MS apparatus; thereby, the C-terminal amino acid sequence of the peptide sample is identified.

The invention discloses a preparation method of 3-hydroxypiperidine, a preparation method of a derivative of 3-hydroxypiperidine, and an intermediate of 3-hydroxypiperidine. The preparation method of 3-hydroxypiperidine (I) is characterized in that 5-halo-2-hydroxypentylamine halogen acid salt (III) undergoes a ring closure reaction in water under the action of an inorganic alkali to obtain the 3-hydroxypiperidine (I). The preparation method of N-protected 3-hydroxypiperidine (II) comprises the following steps: 1, 5-halo-2-hydroxypentylamine halogen acid salt (III) undergoes the ring closure reaction in water under the action of the inorganic alkali to obtain the 3-hydroxypiperidine (I); and 2, the 3-hydroxypiperidine (I) and a nitrogen protection reagent undergo an N-acylation reaction in an organic solvent under the action of the inorganic alkali to obtain the N-protected 3-hydroxypiperidine (II). The preparation methods have the advantages of simple operation, no expensive catalysts, low production cost, easily available raw materials, simplicity in operation, high reaction conversion rate, high selectivity, simple process, and suitableness for industrial production.

The invention relates to a bisamide type ultra-long-life room-temperature phosphorescent compound and a preparation method and application thereof. Four pure organic room-temperature phosphorescent molecules with ultra-long service life are prepared by one-step reaction of N acylation of carbazole and acyl chloride, and thus four compounds, namely, DCED, o-PBCM, m-PBCM and p-PBCM are obtained, andsingle crystals of three compounds DCED, o-PBCM and p-PBCM and floccules of m-PBCM after recrystallization are obtained by using a recrystallization method in an ethanol solution. Compared with the prior art, the four substances obtained by the preparation method have ultra-long service life and room-temperature phosphorescent properties, and particularly, the phosphorescent service life of the compound m-PBCM obtained by the preparation method at room temperature is up to 710.6 ms. When the compound m-PBCM is applied to the field of biology, an m-PBCM nanoparticle solution is injected to theright back of a nude mouse for afterglow imaging, and the signal-to-noise ratio of the m-PBCM nanoparticle solution reaches up to 428; after being injected into a forepaw of a nude mouse, the m-PBCMnanoparticle solution can also be used as an effective afterglow contrast agent to accurately illuminate axillary lymph nodes with excellent sensitivity and signal-to-noise ratio.

The present invention relate4s to an aminoglycoside antibiotic which belongs to the application technology filed of aminoglycoside antibiotic. The present invention provides the derivative of the structure of 2'-NH ₂ -3 ', 4'-deoxy-3'-N demethylase 1-N acylation as well as the application of the derivative in the preparation of medicinal combination in the treatment of drug-resistant virus infections.

The invention provides a set of intermediate compounds used for synthesis of Ivabradine and a preparation method thereof, and also provides a method used for synthesizing Ivabradine from the intermediate compounds. According to the method, the set of intermediate compounds are subjected to a plurality of N alkylation or N acylation so as to obtain a compound IV; and Ivabradine is directly synthesized from the compound IV. The method is short in synthesis route; raw materials are simple and easily available; reaction sequence is reasonable; operation is simple and high in efficiency; the method is green and friendly to the environment; synthesis difficulty of Ivabradine is reduced greatly; cost is low; product yield is high; and the method is suitable for industrialization production.

The invention provides an N-formylation synthesis method taking CO2 as a carbon source under a mild condition and belongs to the technical field of chemistry and chemical engineering. Under normal-temperature and normal-pressure conditions and in a solvent with a low boiling point, CO2 is used as a carbon source to realize N-formylation reaction of various amine type substrates. The N-formylationsynthesis method provided by the invention has the advantages that a reaction system takes sodium borohydride and ammonium sulfate as reaction reagents, and the CO2 is subjected to reduction under normal pressure to provide acyl, so that high-pressure hydrogen gas and toxic CO are not used and reaction conditions are mild; the sodium borohydride and the ammonium sulfate are cheap and easy to obtain and the economic applicability is high; a reagent is stable in the air and is convenient to operate; the organic solvent with the low boiling point is used and is easy to remove and a product is convenient to separate. A method for preparing formamide, provided by the invention, takes greenhouse gas, i.e., carbon dioxide, as a carbon source and has the advantages of relatively low cost, simplicity in operation and mild reaction conditions; the yield of the prepared formamide product is good and a green synthesis method is provided for N-acylation reaction.

The invention belongs to the field of chemical pharmacy and relates to a 7beta-methyl-tetralone derivative shown in a general formula (I) and a preparation method thereof. According to the compound shown in the general formula (I), with thebaine as a raw material, through related conversion methods such as N-demethylation, N-acylation, a Diels-Alder reaction and reduction, oxidation and Grignard reactions, the compound is synthesized. The compound shown in the general formula (I) belongs to an opioid receptor ligand, a radioactive receptor ligand combination experiment is adopted, the affinityand selectivity of the ligand to three subtypes of an opioid receptor are measured, and a [35S]GTPgammaS combination experiment is adopted for measuring the excitement inhibitory activity of the ligand; it is proved through a result that the compound has the functions of alleviating pain, resisting depression, withdrawing opioid addiction, relieving itching and the like and can be applied to preparation of an opioid receptor treatment medicine and applied to clinical analgesia or depression resistance or opioid addiction withdrawal treatment or itching relieving treatment.

The invention discloses a method for preparing an atorvastatin calcium intermediate, and belongs to the technical field of synthesis of medicinal intermediates. The problems that an existing synthesismethod of the atorvastatin calcium intermediate is long in synthesis line and complicated in operation and raw materials are expensive can be solved. By adoption of a 'one-pot' method, firstly, isobutyraldehyde and ATS-9 are condensed to generate imine, and the imine and fluorobenzoyl chloride generate N-acylation reaction and then react with tertiary butyl isonitrile; and finally, the product and 3-phenyl propylene aniline generate 1,3-dipolar cycloaddition-removal reaction to generate a target (4R-cis)-6-[2-[2-(4-fluorinated phenyl)-5-(1-isopropyl)-3-phenyl-4-[( anilino) carboxyl]-1H-pyrrole-1-radical]-ethyl]-2,2-dimethyl-1,3-dioxane-4-tert-butyl acetate. The yield of the final product obtained by the synthesis method disclosed by the invention is as high as 72 to 75 percent.

The invention relates to a method for splitting halogenated alpha-amino acid. According to the invention, after N-acylation of halogenated alpha-amino acid, an acyl group of N-acylated alpha-amino acid with one structure is highly selectively hydrolyzed through selection of a proper enzyme, while a counterpart of the N-acylated alpha-amino acid with the structure does not undergo hydrolysis of acyl group; then separation is carried out based on difference between halogenated alpha-amino acid and N-acyl halogenated alpha-amino acid to obtain optically pure halogenated alpha-amino acid; and optically pure N-acyl halogenated alpha-amino acid undergoes chemical hydrolysis so as to obtain corresponding optically pure halogenated alpha-amino acid. The method provided by the invention has the advantages of stability, environment-friendliness, safety, mild production conditions, capacity of obtaining a product with optical purity as high as 99.9% and low production cost. The method provides a novel approach for industrial production of halogenated alpha-amino acid with high optical purity.

The beta-amino acid resolving process includes the first N acylation of amino acid; hydrolyzing the acyl radical of the N acylated beta-amino acid in some one configuration in high selectivity with properly selected enzyme while not affecting its antimer and extracting according to the difference of different matters in water solubility and fat solubility to obtain one kind of corresponding optically pure beta-amino acid; and hydrolyzing the acyl radical of the N acylated beta-amino acid in one other configuration with one other kind of selected enzyme to obtain one other kind of optically pure beta-amino acid similarly. The said process is stable, environment friendly, safe, low in cost and with mild production conditions, and the product reach optical purity of 99.9 wt%. The present invention provides one new way for producing optically pure beta-amino acid.

The invention discloses a method for preparing beta-amino acid. The method comprises the following steps of: carrying out N acylation on amino acids, making acyl groups of N acylated beta-amino acids of one configuration to be hydrolyzed by enzymolysis to obtain corresponding beta-amino acids and not making N acylated beta-amino acids of a corresponding configuration to be hydrolyzed, separating the above amino acids according to their differences in fat water solubility properties by extraction, choosing another enzyme and hydrolyzing N acylated beta-amino acids of a corresponding configuration to obtain corresponding beta-amino acids, so as to obtain the beta-amino acid of a single configuration. The method provided by the invention is stable, environmentally friendly and safe, requires low cost, and has high optical purity. The invention also provides a new approach to producing optically-pure beta-amino acid.

The invention provides a preparation method of an infrared camouflage textile. The method comprises the following steps: firstly, introducing amino into the surface of aluminum-doped zinc oxide by utilizing low-temperature plasma; then enabling amino on the surface of the aluminum-doped zinc oxide and carboxyl on octacarboxylic metal phthalocyanine to be subjected to N-acylation reaction by utilizing reaction activity of carbodiimide, so as to prepare a phthalocyanine compound/aluminum-doped zinc oxide composite material; then treating the phthalocyanine compound/aluminum-doped zinc oxide composite material on a textile through a coating finishing manner. The textile has a relatively good camouflage effect on near-infrared and mid and far-infrared rays and has washing resistance.