12 results about "Carbamic acid ethyl ester" patented technology

The invention belongs to the technical field of pharmaceutical analysis, and discloses a method for determining two potential genotoxic impurities in carbon [13C]-urea by gas chromatography. Comprising the following steps: (1) preparing a sample solution; (2) preparing a reference solution; (3) taking nitrogen as carrier gas, and detecting by adopting a medium-polarity or weak-polarity chromatographic column separation system; and (4) calculating by a peak area through an external standard method to obtain the accurate contents of methyl carbamate and ethyl carbamate in the carbon [13C]-urea. The method disclosed by the invention is simple to operate, good in specificity, linearity, precision and accuracy and high in sensitivity, and can realize accurate detection of residual potential genotoxic impurities, namely methyl carbamate and ethyl carbamate, in the carbon [13C]-urea.

The invention relates to a method for improving the activity of a Meyerozyma guilliermonii ECH strain for producing ethyl carbamate hydrolase in the technical field of microorganisms, which comprises the following steps: inoculating a bacterial liquid containing the Meyerozyma guilliermonii ECH strain into a liquid fermentation culture medium according to the inoculum size of 10-18%, adjusting the initial pH value to 4-6, and culturing for 3-5 days at the temperature of 25-35 DEG C; the liquid fermentation culture medium contains ethyl carbamate. According to the method, the activity of the strain for producing the ethyl carbamate hydrolase can be remarkably improved.

The invention discloses a novel supramolecular assembly material with nitrogen fertilizer slow release and controlled release functions and a preparation method of the novel supramolecular assembly material, and belongs to the technical field of nitrogen fertilizer synergistic materials. The supramolecular assembly material is prepared from a composite plant source inhibitor, a functionalized hydrogen bond molecule donor, a novel composite dispersing agent and a high-efficiency cosolvent, the composite plant source inhibitor is composed of cyclopentanone, a coumarin derivative and a flavonoid compound. The functionalized hydrogen bond molecular donor is composed of citrulline, N-acetyl urea and ethyl carbamate; the novel composite dispersing agent is prepared from a naphthalene sulfonate formaldehyde condensate, sodium polyepoxysuccinate and nano silicon dioxide; the efficient cosolvent is prepared from acetic acid, acetonitrile and 1-butyl-3-methylimidazole acetate. The supramolecular assembly material is a supramolecular crystal formed by two or more molecules through intermolecular hydrogen bond interaction, and has excellent stability and controllability. After being mixed with a nitrogen fertilizer, the nitrogen fertilizer can be obviously prolonged.

The present application relates to the technical field of genetic engineering and enzyme engineering, and particularly relates to an esterase mutant for degrading ethyl carbamate and application thereof, the esterase mutant has a sequence with site mutation of an amino acid sequence shown as SEQ ID NO. 1, the site mutation is any one or several site combination mutations of V129S, V161L or I229M, wherein the V129S site mutation is that valine at the 129th site is mutated into serine, the V161L site mutation is that valine at the 161st site is mutated into leucine, and the I229M site mutation is that isoleucine at the 229th site is mutated into methionine. The present application is mutated by a method of site-directed mutagenesis, so as to change the amino acid sequence, realize the change of protein structure and function, and finally obtain the esterase mutant V129S / I229M with the hydrolysis rate of ethyl carbamate in an acidic environment increased to 6.55 times, which has high industrial application value.

The invention belongs to the technical field of medicines and medicines, and relates to a preparation method of an upatinib intermediate, which comprises the following steps: reacting N-[5-(4-methylphenyl) sulfonyl]-5H-pyrrolo [2, 3-B] pyrazine-2-yl] ethyl carbamate with (3R, 3R, 3R, 3R, 3R, 3R, 3R, 3R, 3R, 3R, 3R, 3R, 3R, 3R, 3R, 3R, 3R, 3R, 3R, 3R, 3R, 3R The preparation method comprises the following steps: reacting (4S, 4S)-3-(2-bromoacetyl)-4-ethyl-1-pyrrolidine carboxylic acid benzyl ester to prepare the upatinib intermediate. Compared with the prior art, the yield and the purity of the prepared product are greatly improved, the safety of the medicine is improved, and the preparation method is suitable for industrial mass production.

The present application relates to the preparation method of fire-retardant, light-resistant, low VOC, easily permeable water-based polyurethane coating, polytetrahydrofuran ether diol, polyol are added in the reaction container, after mixing, stirring and drying 1~2h to remove water, cooling, adding isophorone diisocyanate, dibutyltin dilaurate, stirring under the condition of 85~95℃ for 1~2h, polyurethane prepolymer is obtained; hyperbranched flame retardant is added to the polyurethane prepolymer for primary chain extension, stirring reaction, the system is cooled, dimethylol propionic acid is added for secondary chain extension reaction, cooling, adding alkyl glycoside, adding char former, stirring for 1h, adding triethylamine, adding acetone, stirring to reduce viscosity, after reducing to 25~30℃, adding water, adjusting the speed of stirrer to 2000r / min, adjusting pH to 7, adding saturated sodium bisulfite and ethyl carbamate, reacting at room temperature, filtering and precipitating, adjusting pH to 7~8, the fire-retardant, light-resistant, low VOC, easily permeable water-based polyurethane coating is obtained, the obtained polyurethane has the advantages of fire-retardancy, low VOC and light resistance.

The invention relates to the field of drug synthesis, and discloses a preparation method of 4-methylbenzenesulfonylurea, which comprises the following steps: (1) adding 4-methylbenzenesulfonamide and alkali into ethyl carbamate for nucleophilic substitution reaction to obtain a 4-methylbenzenesulfonylurea salt crude product; or, adding the 4-methyl benzenesulfonamide salt into ethyl carbamate, and carrying out nucleophilic substitution reaction, so as to obtain a 4-methyl benzenesulfonylurea salt crude product; (2) carrying out purification treatment on the 4-methylbenzenesulfonylurea salt crude product to obtain a 4-methylbenzenesulfonylurea salt clean product; and (3) carrying out acidizing treatment on the 4-methylbenzenesulfonylurea salt clean product to obtain the 4-methylbenzenesulfonylurea. The process route has the advantages of low cost and high product purity, large-scale continuous production of 4-methylbenzenesulfonylurea is realized, and the synthetic method is low in risk, controllable in cost and stable in quality.

The application discloses a synthetic method of eticaptide, belongs to the technical field of polypeptide synthesis, and particularly relates to a synthetic method of eticaptide. The synthetic method comprises the following steps: taking a polypeptide synthesis carrier as a starting material, sequentially reacting with amino acids to perform coupling, performing cleavage treatment through a trifluoroacetic acid cutting liquid, and then reacting with H-Cys-OH.HCl to obtain eticaptide. The polypeptide synthesis carrier is obtained by the following steps: first, reacting 4,4'-dihydroxybenzophenone with a halogen compound, then performing reduction treatment, then reacting with ethyl carbamate, and finally performing sodium hydroxide treatment. The halogen compound is selected from C10-30 straight-chain or branched-chain alkanes containing halogen substituents, wherein the halogen is bromine, chlorine, fluorine or iodine. The eticaptide prepared by the synthetic process has high yield and high purity, the synthesis efficiency and the purification efficiency of the eticaptide are significantly improved, and the eticaptide has a good application prospect.

The invention provides a preparation method of an upatinib intermediate chiral impurity, which comprises the following steps of: dissolving (3R, 4S)-3-(2-bromoacetyl)-4-ethyl-1-pyrrolidine carboxylic acid benzyl ester in an organic solvent 1, reacting with N-[5-[(4-methylphenyl) sulfonyl]-5H-pyrrolo [2, 3-B] pyrazine-2-yl] ethyl carbamate dissolved in the organic solvent 1 under the action of alkali, and reacting at room temperature to obtain the upatinib intermediate chiral impurity. Carrying out nucleophilic substitution reaction at the temperature of 10 DEG C below zero to 0 DEG C to obtain an upatinib intermediate chiral impurity crude product; and recrystallizing the crude product of the upatinib intermediate chiral impurity through an organic solvent 2 to obtain the high-purity upatinib intermediate chiral impurity. The preparation method is simple, efficient, high in yield and high in purity, the impurity can be used for preparing the high-purity upatinib chiral impurity reference substance, and the preparation method has profound significance in quality control of upatinib bulk drugs and preparations thereof.

The invention discloses a synthesis method of Itecatide, belongs to the technical field of polypeptide synthesis, and particularly relates to a synthesis method of Itecatide. The synthesis method comprises the following steps: by taking a polypeptide synthesis carrier as an initial raw material, sequentially reacting with amino acid for coupling, carrying out cracking treatment through trifluoroacetic acid cutting liquid, and then reacting with H-Cys-OH.HCl to obtain the Itecatide, the polypeptide synthesis carrier is prepared by the following steps: reacting 4, 4 '-dihydroxybenzophenone with a halogen compound, carrying out reduction treatment, reacting with ethyl carbamate, and treating with sodium hydroxide. The halogen compound is selected from C10-30 straight-chain or branched-chain alkane containing halogen substituent groups, and halogen is bromine, chlorine, fluorine or iodine. The Itecatide prepared by adopting the synthesis process provided by the invention is high in yield and high in purity, the synthesis efficiency and purification efficiency of the Itecatide are remarkably improved, and the Itecatide synthesis process has a good application prospect.

The invention relates to the technical field of organic catalytic synthesis, and particularly discloses synthesis of an upatinib base fragment, through a catalytic system composed of palladium and phosphine ligands, the catalytic efficiency is remarkably improved, the production cost is greatly reduced, the palladium center is greatly activated through the unique electronic effect and steric hindrance characteristics of the ligands, and the yield of the upatinib base fragment is improved. Compared with the prior art, the method has the advantages that the rate of oxidative addition and reduction elimination is remarkably increased, the dosage of the catalyst is reduced to 0.05 mol%, the consumption of expensive noble metal is greatly reduced, the cost of raw materials is remarkably reduced, the treatment pressure of metal residues is relieved, the excellent yield of 95% or above can still be obtained under the condition of low palladium catalyst loading capacity, the reaction selectivity is extremely high, the reaction conditions are mild, and the method is suitable for industrial production. The method is simple in operation, friendly to operators and suitable for coupling of tert-butyl carbamate and coupling of ethyl carbamate, and a flexible and efficient universal solution is provided for different synthesis process routes of upatinib.

The application provides a synthesis method of tolfenpyrad, and belongs to the technical field of medicine synthesis. Methylamine aqueous solution is used for synthesizing methylaminoformic acid ethyl ester with diethyl carbonate. N-[3-methyl-4-(4-trifluoromethylsulfanyl-phenoxy)-phenyl]-urea (arylurea) is used as a starting material to react with the obtained methylaminoformic acid ethyl ester under the action of a catalyst to synthesize biuret. The biuret is subjected to ring closing with diethyl carbonate to generate tolfenpyrad. The synthesis method does not need to use phosgene, is simple to operate, raw materials are easy to obtain, cost is low, and the yield is high.