34 results about "Chloracetone" patented technology

The preparation method for 2- methyl -3-hydroxyl -6- isopropylquinoline-4- hydroxy acid, which comprises: adding chloral and inorganic salt liquid into reaction bulb, as well as p-isopropoxyphenylamine and strong hydrochloric acid and hydroxylamine hydrochloride, obtaining 4-isopropyloximinoacetamide solid; adding strong sulphuric acid, heating, stirring, cooling; pouring reaction liquid into ice water, filtering to obtain 5- isopropyl-isatin solid; with calcium oxide or calcium hydroxide, adding 5- isopropyl-isatin solid into reaction bulb, heating, dropping chloracetone; then neutralizing with acid to obtain golden-ocher product. This invention is simple and security.

The invention relates to compounds. Cyanoethyl acetate and chloroacetone with different substituent groups are used as initial raw materials, a cyanoethyl ester compound is generated under the action of sodium ethoxide, then furan compounds are generated through intramolecular ring closing under the action of trifluoroacetic acid, the furan compounds respectively react with 2-pyrrolidone, valerolactam and caprolactam under the action of phosphorus oxychloride to form a ring, so as to obtain furo[2, 3-d]pyrimidinone compounds, and then oxygen-sulfur exchange is performed under the action of phosphorus pentasulfide, so as to obtain the furo[2, 3-d]pyrimidinethione compounds. The 54 kinds of obtained tricyclic furo[2, 3-d]pyrimidone compounds are used as positive control of DOX, the inhibitory activity of Hela cervical cancer cells, MCF-7 breast cancer cells and A549 lung cancer cells is achieved, and results show that the compounds C11 and C17 have the inhibitory activity of the Hela cervical cancer cells; the compounds D5 and D7 have inhibitory activity on A549 lung cancer cells; and the compound C14 has inhibitory activity on MCF-7 breast cancer cells.

The invention provides a method for preparing deuterated chloroform by using hexachloroacetone as an intermediate. The method comprises the following steps: step 1, producing hexachloroacetone by monochloroacetone and / or polychlorinated acetone raw material liquid, and comprising the steps of raw material liquid pre-treatment, chlorination catalytic reaction and reaction product purification; step 2, producing deuterated chloroform by taking hexachloroacetone as raw material, and comprising the steps of hydrolytic catalytic reaction and reaction product purification. The method solves the problem of the disposing of waste material produced during the production of monochloroacetone, trichloroacetone and the like, and is in favor of relieving the environment burden; common cheap chemical is used as catalytic agent, the side reaction is less, the reaction product is easy to separate, and the content of the produced pollutant is greatly lowered. Through the utilization of the polarization and weakening effects of connecting bond of the carbonyl carbon of the hexachloroacetone and trichloromethyl, the carbonyl carbon of the hexachloroacetone and trichloromethyl are hydrolyzed in an alkalescence condition to produce deuterated chloroform, and the reaction product is CO2 that can be discharged into air directly. The method has important social benefits and economic benefits.

The invention discloses a synthesis method of a febuxostat decarboxylation impurity, which comprises the following steps: by taking p-hydroxybenzenesulfamide as a raw material, carrying out reflux condensation on p-hydroxybenzenesulfamide and chloroacetone in ethanol, and carrying out hydroformylation, cyanation and alkylation on trifluoroacetic acid and urotropine, so as to obtain the febuxostat decarboxylation impurity with the reaction yield of more than 90% in each step. According to the synthesis method of the febuxostat decarboxylation impurity, the reaction steps are mild and controllable, the operation is simple, and the product purity reaches 99% or above.

The invention discloses a preparation method of tralopyril, and particularly relates to the technical field of agriculture. The preparation method provided by the invention comprises the steps of 1, dissolving p-chlorobenzonitrile in acetonitrile, and carrying out a salt forming reaction under the catalysis of an organic base to obtain an alkali metal salt (I) of p-chlorophenyl amino acrylonitrile; 2, dissolving 1, 1, 1-trichloroacetone in alkyl chloride, carrying out a one-step bromination reaction with bromine, and carrying out extraction and distillation to obtain 1-bromo-3, 3, 3-trifluoroacetone (II); 3, dissolving the intermediate I in alkane, carrying out a ring closing reaction with the intermediate II through acid catalysis to obtain a 2-(4-chlorphenyl)-5-(trifluoromethyl)-1H-pyrrole-3-nitrile crude product, and carrying out distillation and recrystallization to obtain a pure product; and 4, performing two-step bromination on the intermediate III through bromine to obtain tralopyril. According to the intermediate obtained by the preparation method disclosed by the invention, the final product tralopyril is low in impurity content and high in product purity, the raw materials are simple and easy to obtain, the preparation process is simple, the reaction conditions are mild, and the preparation method is economical and environment-friendly and meets the requirements of industrial mass production.

Belonging to the technical field of medicine synthesis, the invention relates to a method for synthesis of PMPA by combining a biological technique and a chemical technique. The method comprises: taking chlorinated acetone as a starting raw material, conducting yeast fermentation reduction so as to obtain chiral chloropropanol (I), then subjecting the chiral chloropropanol (I) and diethyl p-toluenesulfonyloxyphosphonate to a condensation reaction under the action of alkali so as to obtain a reaction intermediate (II); preparing R-9-(2-hydroxypropyl)adenine (III) from adenine and the reaction intermediate (II); and hydrolyzing the obtained R-9[2-(diethylphosphonomethoxy)propyl]purine, thus obtaining the PMPA (IV). The method combines the biological technique and the chemical technique and obtains a key chiral alcohol by means of a biological means, i.e. fermentation. The method has the characteristics of short reaction process, short reaction time, high mass yield, and can produce products with good quality, thus being suitable for industrialized production.

The present invention relates to a kind of synthetic method of 2-methyl-3-hydroxyquinoline and the preparation method of quinone disperse dye; in the synthetic method of 2-methyl-3-hydroxyquinoline, first anthranil , chloroacetone, alkali catalyst, phase transfer catalyst and solvent are mixed, and the pH value is adjusted to 11-13. Under the action of the phase transfer catalyst, each raw material is fully contacted to obtain a uniformly mixed homogeneous mixed solution with a specific pH value; Then the mixed solution is subjected to a microchannel reaction. During the microchannel reaction, the reaction materials in the mixed solution can undergo micron or millimeter level micro-contact reactions, which improves the reaction speed and reaction selectivity, and reduces the amount of ortho-amino groups in the microchannel reaction process. The possibility of benzaldehyde or chloroacetone undergoing self-condensation, thereby improving the yield of 2-methyl-3-hydroxyquinoline.

The invention relates to a method for purifying hexachloroacetone, belonging to the technical field of organic chemical purification. At 8.0KPa ~ 20KPa, after heating the crude hexachloroacetone solution to 45°C ~ 75°C, spray from top to bottom with the purification gas flowing from bottom to top heated to 35°C ~ 75°C for convective interactive contact purification, The low-boiling impurities are separated from the crude hexachloroacetone solution by purifying gas to obtain hexachloroacetone solution; the purifying gas is inert gas or nitrogen; and the low-boiling impurities are mainly pentachloroacetone and tetrachloroacetone. The method has a low material heating temperature, the purified gas can be recycled, the processing capacity can be enlarged, the operation is simple, and hexachloroacetone with extremely low impurity content can be obtained.

The invention discloses a method for preparing pymetrozine with an aim to provide a synthesis method short in reaction route of the pymetrozine, small in environmental pollution and simple in technology operation, and belongs to the technical field of organic synthesis. The method includes the steps of 1), allowing dimethyl carbonate serving as a raw material to be subjected to hydrazinolysis withhydrazine hydrate to obtain carbazide; 2), subjecting carbazide and smoke aldehyde to condensation reaction to obtain (E)-N'-(pyridine-3-kiya methyl) hydrazine carbon hydrazide; 3), subjecting (E)-N'-( pyridine-3-kiya methyl) hydrazine carbon hydrazide and chloroacetone to condensation reaction to obtain (E)-N'-(Z)-1-chloropropyl-2-subunit)-2-(pyridine-3-kiya methyl) diazanyl-1-carbohydrazide; 4), subjecting (E)-N'-(Z)-1-chloropropyl-2-subunit)-2-(pyridine-3-kiya methyl) diazanyl-1-carbohydrazide to ring formation under the alkaline condition to obtain the pymetrozine.

The invention discloses a method for synthesizing 2, 4-dimethyl pyrimidine-5-alcohol serving as an intermediate of Lemborexant , and aims to solve the problems of safety risk and heavy environmental pollution of the 2, 4-dimethyl pyrimidine-5-alcohol in industrial production of the 2, 4-dimethyl pyrimidine-5-alcohol. The preparation method comprises the following steps: firstly, carrying out esterification reaction on benzoic acid serving as an initial raw material and chloroacetone; then, carrying out alkylation reaction and ring closing reaction with N, N-dimethylformamide dimethyl acetal and acetamidine hydrochloride; and finally, carrying out hydrolysis reaction to remove benzoic acid to obtain the 2, 4-dimethyl pyrimidine-5-alcohol. According to the method, benzoic acid widely existing in nature serves as a main raw material, the health problem caused in production is solved, the raw materials are non-toxic, and the method has the advantages that the EHS risk is low, the cost is low, the production efficiency is high, the yield is larger than or equal to 60%, and the purity is larger than or equal to 99.0%.

The invention discloses a method for preparing lorcaserin. Specifically, the method comprises the steps: taking p-chlorophenylacetonitrile as an initial raw material, preparing p-chlorophenylethylamine through reduction; carrying out a reaction with p-toluenesulfonyl chloride to form an amino occupying intermediate; enabling the intermediate to carry out a reaction with monochloroacetone under analkaline condition to form N-(2-(4-chlorphenyl)ethyl)-4-methyl-N-(2-propionyl)benzenesulfonamide, and then carrying out reduction, chlorination, p-toluenesulfonyl removal and intramolecular Friedel-Crafts alkylation to synthesize 8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzoazepine, carrying out L-(+)-tartaric acid resolution and alkalization on azepine to remove tartaric acid, and acting with hydrogen chloride diethyl ether to salify to prepare lorcaserin. The method has the characteristics of simple synthesis method, good reaction selectivity, high product purity, environmental protectionand low preparation cost.

The invention relates to a simple synthesis method of a 2-aminothiophene derivative. The method comprises the steps of condensating monochloroacetone, alkyl / aryl-piperzine under the effect of inorganic base to prepare a piperzine derivative II, mixing the piperzine derivative II with 4-chlorobenzoyl acetonitrile and sulphur, dropping organic amine, performing heat preservation reaction, and reacting in two steps to obtain 2-amino-3,(4- chlorine)-benzoyl-4-(N- alkyl / aryl-piperzine-N '-) methylthiophene. The simple synthesis method of the 2-aminothiophene derivative is available in raw materials, simple to operate, simple in synthesis steps and environmental-friendly; meanwhile, products are high in selectivity, yield and purity and applicable to industrial application.

The invention provides a 1,1,1-trichloroacetone preparation method, which comprises the following steps: 1, adding monochloroacetone and an alkaline compound into a large amount of an aqueous solutionwithout other organic solvents; 2, forming an aqueous solution or a turbid liquid from the alkaline compound in water while stirring; 3, introducing chlorine gas while stirring until the solution isclear; and 4, in the whole reaction process, controlling the temperature at 0-25 DEG C. According to the invention, the method is simple in process, convenient to operate, high in yield and convenientfor industrial production, and can effectively control the acetone chlorination position, so that the generation of byproducts such as 1,1,3-trichloroacetone, tetrachloroacetone, pentachloroacetone and the like is reduced, and the purity of the prepared product is high and can reach more than 85% without further purification.

The invention relates to a preparation method of hexachloroacetone, which belongs to the technical field of organic chemical gas preparation. Compound A and chlorine molecule B are mixed and reacted at 30°C to 150°C under the action of a catalyst, and the reaction product is a mixture containing hexachloroacetone and the catalyst; the catalyst is separated from the mixture to obtain a crude product; the crude product is purified to obtain Hexachloroacetone; compound A is at least one of acetone and chloroacetone with chlorine atoms of 1 to 5; chlorine molecule B is a mixture of chlorine or chlorine and a diluent gas, and the diluent gas is an inert gas or nitrogen; the catalyst is pyrimidine, 2-chloropyrimidine, 2-cyanopyrimidine or s-triazine. The method is easy to recover the catalyst, and can obtain the hexachloroacetone with extremely low impurity content in high yield.

The present invention relates to a production method of hexachloroacetone, including performing a reaction between at least one kind of compound (A) selected from the group consisting of acetone and chloroacetones having a chlorine atom number of from 1 to 5, and a chlorine molecule (B) in a solvent in the presence of an activated carbon, to obtain the hexachloroacetone.

Epichlorohydrin is produced from acetone by (1) chlorinating acetone to form monochloroacetone; (2) disproportionating the monochloroacetone in the presence of a platinum catalyst, a strong acid and preferably a chloride source (for example, added as a salt or from hydrolysis of monochloroacetone) and some water to produce acetone and 1,3-dichloroacetone; (3) hydrogenating the 1,3-dichloroacetone in the presence of a catalyst to produce 1,3-dichlorohydrin; and (4) cyclizing the 1,3-dichlorohydrin with a base to produce epichlorohydrin.

The invention discloses a method for purifying high-purity trichloroacetone for preparation of folic acid. The method is characterized in that a water solvent is used for purifying to prepare the high-purity trichloroacetone, and comprises the following steps of step 1, using the water solvent to extract the trichloroacetone with purity of 50% by three times; step 2, recrystallizing the obtained extracting solution by a gradient cooling type, and increasing the purity of the crude trichloroacetone with purity of about 50% to be above 98% by two steps of purification, wherein the extracting yield rate of trichloroacetone is 90% or above, the solution after separating and crystallizing in step 2 can be repeatedly utilized, and the yield rate of trichloroacetone can reach 80% or above by raw material. The method has the advantages that the preparation of high-purity trichloroacetone is easy, the safety and environment-friendly effects are realized, and the requirement of industrialization on environment protection is met; the prepared high-purity trichloroacetone can be used for preparing the folic acid, and the yield rate and purity of the folic acid are certainly improved.

The invention discloses a preparation method of a CDK (Cyclin-dependent Kinase) inhibitor. The preparation method comprises the following steps: enabling monomethylthiourea and 1-chloroacetone to react to obtain N,4-dimethylthiazole-2-amine; carrying out bromination reaction to obtain 5-bromo-N,4-dimethylthiazole-2-amine; enabling the 5-bromo-N,4-dimethylthiazole-2-amine and borate to react under the action of a catalyst, so as to obtain an aromatic borate intermediate; enabling the aromatic borate intermediate and 2,4-dichloro-5fluorouracil to be subjected to suzuki coupling reaction under the catalysis of a palladium series catalyst, so as to obtain a coupled product; enabling the coupled product and aromatic amine to be subjected to Buchwald-Hartwig reaction to finally obtain a target product.

The invention relates to a preparation method of 2,4,5-triamino-6-hydroxypyrimidine sulfate and folic acid. The preparation method comprises the following steps: enabling cyanoacetate and sodium nitrite to be subjected to reaction under the action of an organic solvent and / or an inorganic solvent and an acidic substance to obtain 2-oximidocyanoacetate; then, enabling the 2-oximidocyanoacetate andguanidine hydrochloride to be subjected to reaction under an alkaline condition to obtain 2,4-diamino-5-isonitroso-6-oxopyrimidine; enabling the 2,4-diamino-5-isonitroso-6-oxopyrimidine and hydrogen gas to be subjected to reaction under an alkaline condition by means of action of Pd / C to obtain 2,4,5-triamino-6-hydroxypyrimidine, and adding sulfuric acid to adjust the pH value to obtain 2,4,5-triamino-6-hydroxypyrimidine sulfate; and then, adding trichloroacetone and N-(4-aminobenzoyl)-L-glutamic acid to be subjected to reaction in a buffer solution under the action of a catalyst molecular sieve so as to obtain the folic acid. Based on the process route, the invention explores the influences of different reaction steps and refining conditions on the preparation route of 2,4,5-triamino-6-hydroxypyrimidine sulfate and the folic acid so as to reduce the wastewater pollution while increasing the yield.

The invention relates to the field of organic synthesis and discloses a method for preparing 1,1,3-trichloroacetone. The method comprises: in the presence of an acidic catalyst, contacting a raw material containing 1,1-dichloroacetone and / or 1,3-dichloroacetone with symclosene for reaction. The method for preparing 1,1,3-trichloroacetone provided by the invention can achieve the purpose of obtaining 1,1,3-trichloroacetone with high purity and high yield in a short period in a pilot production process or even an industrial production process.

The invention discloses a hydrodechlorination device and method for trichloroacetone, relates to the technical field of chemical purification, and comprises a reaction vessel and a base, the reaction vessel is placed above the base, and the reaction vessel is provided with a first bottle opening, The second bottleneck, the third bottleneck and the fourth bottleneck, the second bottleneck is located at the center position, and a stirring structure is arranged in the second bottleneck; the stirring mechanism includes a stirring rod, a stirring rod arranged on the outside The end cover plug, the sliding sleeve, the stirring blade arranged at the bottom of the stirring rod and the connecting rod rotatably connected with the stirring blade, the feeding structure is arranged inside the stirring rod, and the upper end of the stirring rod is connected with the driving mechanism. This invention eliminates the The magnetic stirring bar interferes with the tubes in the reaction vessel when rotating, and improves the stirring efficiency at the same time, which is suitable for batch dechlorination treatment; and the stirring blades are easy to extend and retract, which is convenient for installation and disassembly.