420results about How to "Short reaction steps" patented technology

The invention provides a 3-methylamine tetrahydrofuran preparation method, wherein 1,4-butenediol is adopted as a raw material and is subjected to cyclization dehydration under the catalysis effect of a solid acid to produce 2,5-dihydrofuran, the 2,5-dihydrofuran reacts with water gas under the catalysis effect of cobalt acetate to produce 3-tetrahydrofuran formaldehyde, and the 3-tetrahydrofuran formaldehyde, ammonia gas and hydrogen gas are subjected to a hydrogenation reaction under the catalysis effect of 5% Pd/C to prepare the target product3-methylamine tetrahydrofuran, wherein the purity is 98.12%, and the total yield is 74.16%. According to the present invention, the preparation method has advantages of cheap and easily available raw materials, less steps, simple operation, high product purity, high yield, less three-waste pollution and production cost reducing, and is suitable for industrial production.

The invention relates to a preparation method of Agomelatine, which aims at economically preparing the Agomelatine on a large scale. The preparation method is characterized by comprising the following steps of: carrying out the dehydrogenation on a compound in a formula (I) under the action of DDQ to obtain a compound in a formula (II), reducing the compound in the formula (II) by sodium borohydride to obtain a compound in a formula (III), and reacting the compound in the formula (III) with acetylchloride to obtain a compound in a formula (IV), that is to say, the compound in the formula (IV) is the Agomelatine.

The invention relates to a preparation method of 4-(2, 3-dichlorophenyl)-2, 6-dimethyl-1, 4-dihydro-5-methoxylcarbonyl-3-pyridinecarboxylic acid (I). The method is characterized in that methyl acetoacetate, stronger ammonia water and 2, 3-dichlorobenzaldehyde are used as raw materials for direct cyclic condensation to obtain 4-(2, 3-dichlorophenyl)-2, 6-dimethyl-1, 4-dihydro-3, 5-pyridinedicarboxylic acid methyl ester (II); part of the compound II is hydrolyzed under alkaline condition to obtain the product 4-(2, 3-dichlorophenyl)-2, 6-dimethyl-1, 4-dihydro-5-methoxylcarbonyl-3-pyridinecarboxylic acid (I). The method has the advantages that the starting materials are cheap and easy to obtain, the production cost is lowered, the reaction is easy to operate and industrialization is easy to realize.

The invention discloses a method for preparing lenalidomide. The method comprises the following steps: firstly, etherifying 2-methyl-3-nitrobenzoic acid to obtain 2-methyl-3-nitrobenzoic acid methyl ester, brominating to obtain 2-brooethyl-3-nitrobenzoic acid methyl ester, reacting L-glutamine and tert-butyl dicarbonate to obtain N-Boc glutamic acid, acquiring 3-amino-2,6-piperidine diketone protected by Boc from N-Boc-glutamic acid in the presence of a condensing agent and a catalyst, further reacting with acid to prepare 3-amino-2,6-piperidine diketone hydrochloride, reacting 3-amino-2,6-piperidine diketone with 2-brooethyl-3-nitrobenzoic acid methyl ester so as to obtain 3-(4-nitryl-1,3 dihydro-1-oxo-2 hydrogen-isobenzazole-2-yl) piperidine-2,6-diketone, and finally reducing, thereby obtaining lenalidomide. The method disclosed by the invention is high in product yield.

The invention relates to the field of pharmaceutical chemistry, in particular to a synthesis method of a minodronate midbody and synthesis of minodronate. The preparation method of minodronate includes the following steps: using organic solvent to dissolve 2-aminopyridine, adding 4-acetyl chloride ethyl acetoacetate for reaction, monitoring the reaction solution by TLC(Thin-Layer Chromatography) until spots of 4-acetyl chloride ethyl acetoacetate disappear, concentrating to a dry state, dissolving concentrate in water, washing a water layer to remove impurities, extracting the water layer with the organic solvent, washing extract liquor, separating out an organic layer, conducting filtration, and concentrating the concentrate to be in a dry state, thereby obtaining A1.

The invention explores a method for synthesizing and refining cinacalcet hydrochlorid, especially avoids toxic and expensive reaction reagents reported in literatures; the invention has the advantages of convenient sources of raw materials and reagents, low cost, little pollution to environment and simple operation, the invention is suitable for industrial production.

The invention discloses a production technology for synthetizing salbutamol sulphate, and relates to the field of chemical synthesis. The production technology comprises the following steps: firstly, performing an Friedel-crafts acylation reaction on salicylal to obtain a chemical compound 3, performing a substitution reaction of tert-butylamine, protecting dihydroxy by propylidene under the catalysis of concentrated sulfuric acid through the reduction of potassium borohydride or sodium borohydride, then performing extraction for desalting, and generating a hydrolysis reaction under acid conditions to obtain sulphuric acid salbutamol. The production technology disclosed by the invention is easy to control and operate, raw materials are simple and easy to obtain, the total mol yield is as high as 40%, the product purity is as high as 99.5%, and the product cost is low.

The invention relates to generation of a sodium dihydroxyl sulfonate compound by a substitution reaction of a saturated aqueous solution of sodium sulfite and a chloro dihydroxy compound; a dehydration reaction is carried out for the sodium dihydroxyl sulfonate compound obtained by the step and excess dehydrating agents, after the reaction, excess dehydrating agents are removed; residual sodium dihydroxyl sulfonate is removed by washing and extracting the reaction products; drying and purification are carried out in order to obtain a hydroxy substituted sultone compound; a fluorination reaction is carried out for the obtained hydroxy substituted sultone compound and a fluorating agent, underpressure distillation and purification are carried out, and the fluorosultone compound is obtained. The method has the advantages of cheap raw material, easy purchase, simple operation steps, mild reaction conditions, short reaction steps, easy purification, and high purity of produced products.

The invention discloses a synthesis method of vinpocetine, comprising the following steps: adding vincamine into a three-opening bottle, subsequently, adding methylbenzene, stirring and dropwise adding triethylamine and methylsufonyl chloride in an ice-water bath, slowly heating to room temperature after stirring for 2 h, then continuously stirring for 5 h; stopping reaction, drying solvent by distillation, adding ethanol and water, regulating pH to 12 with saturated potassium carbonate solution, separating out solids, filtering, and drying in vacuum to obtain vinpocetine intermediate; adding absolute ethyl alcohol into the three-opening bottle, stirring in ice-water bath for 1 h, then slowly adding sodium ethoxide, stirring for 0.5 h, then adding the vinpocetine intermediate, subsequently, putting a reaction bottle into an oil bath, setting temperature as 80 degrees centigrade, evaporating most of solvent after reacting for 12 h, then pouring solution into hydrochloric acid, extracting with ethyl acetate, regulating pH to 12 with water phase, separating out solids, filtering and drying to obtain the vinpocetine. According to the synthesis method provided by the invention, reaction steps are short; purity and yield of products are high; energy consumption is low; and environmental pollution is less.

The invention relates to a method for preparing N-dimethylamino propyl methacrylamide by catalyzing and cracking, which comprises the following technical steps: A. two incipient ingredients methyl methacrylate and N, N-dimethyl-1, 3-propane diamine are sealed in an autoclave for catalyzing and condensing, so as to generate the intermediate N-dimethylamino-Beta-dimethylamino methacrylamide; B. putting the intermediate N-dimethylamino-Beta-dimethylamino methacrylamide into a reactor with distilling apparatus and driving off the crude products of N-dimethylamino propyl methacrylamide through catalyzing and cracking; C. adding the crude products of N-dimethylamino propyl methacrylamide and polymerization inhibitor into a rectifying tower to generate the finished products. The invention has the advantages of less reaction steps, high conversion rate, small amount of byproducts, low cost for post treatment, and ability to meet application demand.

The invention provides a preparation method suitable for industrially producing oteracil potassium. The method provided by the invention has the advantages that: reaction steps are fewer, oxidants which generate gases polluting the environment are not used, a refining method is simple, the consumption of organic solvents which are harmful to the human body is decreased, the cost is saved, the total yield can reach more than 65%, and the method is suitable for the industrial production; the purity of a product reaches more than 99.8%, the impurity content of the single product is less than 0.1% and the purity and the impurity of the product both reach quality standards for the raw material medicine; and the obtained product is the oteracil potassium raw material medicine which is suitable for preparation of a medicinal preparation.

The invention relates to a preparation method of carbazochrome sodium sulfonate, belonging to the technical field of preparation of vascular hemostatics. The method comprises the following steps: raw materials dissolution and reaction: putting purified water, carbazochrome, sodium bisulfite and ascorbic acid into a reaction tank, heating while stirring until the solid substances are completely dissolved, and continuing keeping the temperature to react, thereby obtaining a reaction solution; decolorization and separation: adding a decolorant into the reaction solution, keeping the temperature while stirring for decolorization, after finishing decolorization, carrying out centrifugal filtration, washing residues with purified water, carrying out centrifugal drying, and merging the centrifugal filtrates to obtain a solution to be crystallized; crystallization: regulating the pH value of the solution to be crystallized with an alkaline matter, freezing to cooling, and standing to precipitate crystals; and refinement: carrying out centrifugal filtration on the crystals, washing, carrying out centrifugal drying, and drying in a vacuum drying oven to obtain the carbazochrome sodium sulfonate. The invention has the advantages of accessible reaction raw material, short reaction steps, mild reaction conditions, high reaction yield (up to more than 90%), better reaction product quality and high purity (up to more than 99%), and is convenient and simple to operate.

The invention belongs to the field of organic synthesis and particularly relates to a method for preparing DMAPPA (N-(3-dimethyl aminopropyl) acrylamide) through catalytic amidation. According to the method, methyl acrylate, N,N-dimethyl-1,3-propanediamine, a catalyst and an inhibitor are added to a reaction kettle, stirred, heated and cooled, excessive solvent is steamed out, an intermediate product is subjected to reduced pressure distillation treatment, then a distillate is added to a fractionating tower, reduced-pressure heating is performed for collection of a product distillate, and DMAPPA with the purity higher than or equal to 98% is obtained. The process developed with the method is simple and convenient to operate, a few reaction steps are included, and the raw material methyl acrylate is low in cost, easy to obtain and convenient to store and transport; methyl alcohol is generated in a reaction process, so that the reaction temperature is reduced, reaction conditions are mild, and side reactions are reduced; the novel catalyst is selected, accordingly, the reaction speed is high, the yield is high, the product quality is good, polymerization in a tower due to high temperature and high material activity in a distillation process is avoided, and three wastes are hardly generated.

The invention belongs to the technical field of chemical drug intermediate preparation and relates to a preparation method of an isavuconazole intermediate. The preparation method is a 4-(2-((2R, 3R)-3-(2, 5-difluorophenyl)-3-hydroxy-4-(1H-1, 2, 4-triazole-1-yl)butane-2-yl)thiazole-4-yl)benzontrile preparation method. The 4-(2-((2R, 3R)-3-(2, 5-difluorophenyl)-3-hydroxy-4-(1H-1, 2, 4-triazole-1-yl)butane-2-yl)thiazole-4-yl)benzontrile has a structural formula (I) shown in the description.

The invention discloses a synthetic method of bempedoic acid. The method comprises the following steps of: taking isobutyronitrile (ester) as a starting raw material, carrying out reaction with 2, 5-dibromopentane under the catalysis of alkali to generate 7-bromo-2, 2-dimethylheptonitrile (ester), then forming a Grignard reagent with magnesium, carrying out reaction with formate to generate 8-hydroxy-2, 2, 14, 14-tetramethylpentadecane dinitrile (ester), and finally carrying out alkaline hydrolysis and acidification to obtain bempedoic acid. The synthetic route is short, all the used raw materials are easy to obtain, the cost is low, the yield of each step of reaction is high, and the purity is high, therefore the method is suitable for industrial production.

The invention discloses a preparation method of 2'-deoxycytidine analogue decitabine (formula I) capable of effectively inhibiting growth of tumour cells. The method comprises the steps of using 1-methyl-2-deoxy-D-ribose (formula II) as initial raw material, subjecting the initial raw material and acetic anhydride to a reaction to obtain 1-methyl-3,5-diacetoxyl-2-deoxy-D-ribose (formula III); subjecting the compound of formula III and 2,4-bi-(trimethyl silicon)-5-azacytosine (formula IV) to a reaction to obtain 3',5'-diacetoxylgroup-5-aza-2'-deoxycytidine (formula V); hydrolysing the compound of formula V under the action of D315 macro-porous weakly basic anion exchange resin to obtain the decitabine (formula I). The raw materials of the invention are easily obtained, the reaction conditions are moderate and the operation is simple and convenient. The preparation method is suitable for commercial production.

The invention relates to a novel method for preparing N- amino-3-DBU [3, 3, 0] octane bromide. The technical problem to be solved is to simplify the preparation process, reduce the pollution and avoid using a carcinogenic substance. The preparing method comprises the following steps that: 1) a substance shown as formula (II) is taken as a raw material and is added with water, the mixture reacts sufficiently with HXO hydrazine at a temperature of between 80 and 200 DEG C to produce the reaction fluid; 2) after the reaction finishes, the reaction fluid is concentrated, water-solubility ethanol is added to dissolve the reaction fluid and to separate out superfluous HXO hydrazine; 3) sediment is filtered; and the mother fluid is processed to produce the N- amino-3-DBU[3, 3, 0] octane bromide.