51 results about "Cyanothymidine" patented technology

The invention discloses a fused cyanopyridine compound shown as a general formula I-1 or I-2, or a pharmaceutically acceptable salt thereof, or an enantiomer, a diastereoisomer, a tautomer, a torsional isomer, a solvate, a polymorphic substance or a prodrug thereof, and a preparation method and a pharmaceutical application of the fused cyanopyridine compound, wherein the definition of each group is shown in the specification.

The invention discloses the use of variovoraxboronicumulans CGMCC 4969 in bioconversion of 3-cyanopyridine for forming nicotinamide. The nitrile hydratase gene cluster produced by the strain consists of a DNA sequence represented by SEQ ID No.1 in a sequence table; the DNA consisting of the sequence represented by SEQ ID No.1 is recombined onto a pET28a plasmid and can be induced to express in EscherichiacoliBL21(DE3) strain; and the Escherichia coli cells containing expressed proteins and cell extracting solution can convert 3-cyanopyridine into nicotinamide.

The present invention provides an ion palladium activation liquid and a preparation method thereof, and a plastic surface chemical plating method. The ion palladium activation liquid comprises a soluble palladium salt, copper chloride, a chloride complexing agent, 1,10-phenanthroline and 4-cyanopyridine, and the pH value of the ion palladium activation liquid is 6-12. According to the present invention, the service life of the activation liquid is long, the plating time of the material activated with the activation liquid is short, no overflow plating or leakage plating phenomenon is generated, and the adhesion is strong.

The invention discloses a preparation method of substituted pyridine. The method is implemented in a jet loop reactor based on a Venturi effect. First nitrogen displacement is performed, then, acrylicacid and 4-cyanopyridine raw materials are sequentially added through a material feeding opening; an outer circulating pump is started at 70 to 110 DEG C for high-speed spraying and mixing; a hydrogen chloride raw material is slowly added into the jet loop reactor through a gas raw material feeding hole; spraying and mixing are performed through a spraying type mixer, and full reaction among materials is realized; and the like. According to the method, a novel jet loop reactor based on the Venturi effect is adopted; a traditional stirred tank reactor is replaced; according to the reactor, themass transfer among various reaction species in the reactor is greatly promoted, so that the reaction can be dynamically controlled, and when reaction raw materials are sprayed and pushed forwards under the action of the pump, strong suction force can be generated to automatically suck gas-phase reaction materials in the reaction kettle, so that an excellent mass transfer effect is obtained in violent turbulent flow.

The invention discloses a method for preparing 6-chlorine-4-trifluoromethyl-3-cyanopyridine. The method comprises steps of synthesizing 2-chlorine-6-methoxy-4-trifluoromethyl-3-cyanopyridine, synthesizing 6-methoxy-4-trifluoromethyl-3-cyanopyridine, synthesizing 6-hydroxy-4-trifluoromethyl-3-cyanopyridine, and synthesizing 6-chlorine-4-trifluoromethyl-3-cyanopyridine. The method has high productivity and short reaction steps, is simple to operate, is efficient and is easy to carry out.

The invention provides a synthesis method of topiroxostat, and relates to the technical field of medicine synthesis. The synthesis method of topiroxostat comprises the steps of carrying out heat-preservation stirring reaction on a raw material 4-cyanopyridine and 80% hydrazine hydrate in the presence of an alcohol solvent and an alkaline reagent, and carrying out post-treatment to obtain an intermediate 1, or carrying out post-treatment under the condition of hydrochloric acid to obtain a hydrochloride form of the intermediate 1; reacting the intermediate 1 or the hydrochloride form of the intermediate 1 with 2-cyano-4-picolinic acid in the presence of a solvent and a condensing agent, and performing post-treatment to obtain an intermediate 2; and heating and refluxing the intermediate 2 for 2-4 hours under the condition of acetic acid, cooling to room temperature, filtering, and carrying out forced air drying to obtain the topiroxostat (crystal form I). The synthesis method has the advantages of low production cost, high yield, high purity and less three wastes, and is suitable for industrial production of topiroxostat and intermediates thereof.

The invention relates to an organic compound taking 4-cyanopyridine as a core and an organic light-emitting device comprising the same, belongs to the technical field of semiconductors, and provides a compound with a structure shown in a general formula (1), and also discloses an organic light-emitting device comprising the compound. The compound provided by the invention has relatively high thermal stability, can generate a TADF effect when being used as a luminescent layer material of an OLED luminescent device, has relatively high PLQY and relatively small spectral change, and can effectively improve the photoelectric property of the OLED device and prolong the service life of the OLED device.

The invention discloses an indium oxide nanosphere coating brevibacterium flavum nitrile hydratase, a preparation method and application. The multilayered structure of cells is simulated by referring to the existence form of the hydratase in a living body, and the indium oxide nanosphere is prepared through bionic design of components, functions and processes and used for embedding of the brevibacterium flavum nitrile hydratase. The characteristics that the immobilized nitrile hydratase is high in stability, high in activity, easy to recycle and the like are used for catalyzing 3-cyanopyridine to be transformed into nicotinamide in an efficient hydrolysis mode. The preparation method of the bionic immobilized hydratase can provide reference significance for preparation of a microcyst immobilized carrier, and provide a novel research idea for biotransformation of the 3-cyanopyridine.

The invention provides a method for separating 4-cyanopyridine through solvent cooling crystallization. The method comprises the following steps: S1, preparing a 4-cyanopyridine saturated solution; S2, cooling the saturated solution to obtain a mixed slurry; S3, carrying out centrifugal filtration on the mixed slurry, washing with pure water, and carrying out centrifugal filtration and drying to obtain highly-pure 4-cyanopyridine; S4, performing reduced pressure distillation on the obtained filtrate to obtain a solute, heating and decolorizing the solute, and repeating step S1 and step S2 to obtain highly-pure 4-cyanopyridine; and S5, collecting the highly-pure 4-cyanopyridine obtained in step S3 and step S4 to obtain the finished 4-cyanopyridine product. The purity of the 4-cyanopyridineseparated through cooling crystallization is high, and reaches up to 99.54%; the primary filtrate and the washing filtrate are distilled and then purified, so the yield of 4-cyanopyridine is increased, and can reach up to 97.2%; and a separation and purification device for 4-cyanopyridine can complete a series of steps of crystallization, centrifugation, washing, drying and the like in separationand purification of 4-cyanopyridine.

The invention provides a synthesis method of 3, 5-dichloro-2-cyanopyridine. The method includes the steps of: 1) in the presence of a solvent, mixing 2, 3, 5-trichloropyridine with a fluoride for reaction to obtain 3, 5-dichloro-2-fluoropyridine; and 2) mixing the 3, 5-dichloro-2-fluoropyridine prepared in step 1) with a catalyst and a cyanide salt for reaction to obtain 3, 5-dichloro-2-cyanopyridine. The method provided by the invention uses sodium cyanide, potassium cyanide or other cheap and easily available cyanide salts as the cyaniding reagent with a dosage far lower than that of the existing method, and can acquire the target product with high yield and high content, thereby greatly reducing the production cost, also greatly reducing the production of wastewater in the three wastes,and being an efficient and environment-friendly production method of 3, 5-dichloro-2-cyanopyridine.

The invention discloses a rectification separation device and method for a 2-cyanopyridine backing material. The method comprises the following steps: pouring a prepared backing material into a heating stirring kettle, driving a stirring shaft and stirring blades to stir by a stirring motor in the heating stirring kettle, and heating in cooperation with a heating resistor, so that ammonia water in the backing material is decomposed into ammonia gas in an accelerated manner; ammonia gas is mixed with other gases and guided into the rectification separation tower through the heat preservation connecting pipe, firstly, the sulfuric acid solution at the bottom of the rectification shell is bubbled through the gas outlet guide pipe, so that the sulfuric acid solution absorbs a large amount of ammonia gas, and meanwhile, a small part of ammonia gas and other gases are upwards absorbed through the filter screen plate, the coarse filter filler and the fine filter filler; and finally, the residual gas is conveyed to the liquefaction assembly through the heat preservation connecting pipe, liquefied through the liquefaction assembly and then guided into the heating stirring kettle again through the conveying pipe, the heating stirring kettle continues to conduct heating and stirring to conduct the next rectification separation cycle, ammonia water in the prepared base material is effectively separated, and the situation that the ammonia water is decomposed into ammonia gas and pollutes the environment is avoided.

The invention belongs to the field of analytical chemistry, and particularly relates to a method for determining the content of 4-cyanopyridine and impurities of 4-cyanopyridine in an isoniazide starting material. The measuring method is a gas chromatographic method, and comprises the following specific steps: vaporizing a sample in a vaporization chamber, and introducing the vaporized sample intoa chromatographic column through flowing gas; separating the 4-cyanopyridine SM1 and the impurities of 4-cyanopyridine by means of programmed heating; calculating the content of the impurities by using a principal component self-contrasted method with a correction factor. At present, no reports of simultaneous separation and determination of a plurality of impurities in the SM1 exist. The methodfor measuring the content of the plurality of impurities in the SM1 provided by the invention is simple and feasible, and has high sensitivity and high specificity, so that established quality controlitems of SM1 relevant substances can improve the quality controllability and safety of a product when being applied to control of relevant substances of the product.

The invention provides a preparation method of 6-chloro-4-trifluoromethyl-3-cyanopyridine, which comprises the following steps: by taking 2-chloro-3-trifluoromethyl acrylate (II) and 2-chloro-3-aminopropionitrile (III) as raw materials, carrying out addition reaction to obtain 2,4-dichloro-3-trifluoromethyl-4-cyano-5-amino valerate (IV), carrying out molecular lactamization reaction to obtain 3,5-dichloro-4-trifluoromethyl-5-cyano piperidine-2-one (V), then removing hydrogen chloride to obtain 6-hydroxy-4-trifluoromethyl-3-cyanopyridine (VI), and then carrying out chlorination reaction on VI and a chlorination reagent to obtain 6-chloro-4-trifluoromethyl-3-cyanopyridine (I). The raw materials used in the invention are cheap and easily available; the preparation and operation method is simple, small in wastewater amount, safe, environment-friendly and low in cost; the method has the advantages of high reaction selectivity, few byproducts and high target product yield and purity, and is suitable for green industrial production.

The invention discloses a preparation method of a medicine for treating chronic hyperuricemia. The method comprises the following steps: using methyl 2-cyanoisonicotinate and 4-cyanopyridine as initial raw materials, and carrying out hydrazinolysis reaction, condensation reaction, cyclization reaction and purification to obtain topiroxostat. On one hand, by using a hydrochloric acid alcohol solution, the energy consumption of the process is reduced, and the problem of poor safety is improved; and on the other hand, topiroxostat hydrochloride is refined and concentrated in alcohol water and then subjected to a salt dissolving process, so that the solubility of the topiroxostat in an alkaline solution is increased, the problem that chloride exceeds the standard is preliminarily solved, the salt dissolving process is more thorough, and the reaction proceeding degree is increased. Finally, in the purification process, the amount of chlorides in the product is further reduced by a method of hot melting the crude product in alcohol water, and the product quality is ensured; and the purity of the product is improved by selecting a purification solvent.

The invention discloses a preparation method of a 2-bromoindolizine derivative. The preparation method comprises the following steps: putting bromoacetophenone-4-cyanopyridine quaternary ammonium salt, bromoethynylbenzene, tetramethyl-1-piperidinyloxy, potassium carbonate and a solvent into a reactor, and reacting at 90 DEG C; and after the reaction is finished, pouring the obtained mixture into water, and carrying out extraction, drying and column chromatography separation to obtain the pure 2-bromoindazine derivative. The used raw materials can be directly purchased, are easy to obtain and are low in price. The used solvent has high boiling point, is non-volatilize and is safe to operate and use. The synthesis method is wide in substrate application range, and synthesis of the target product with various structures is easy to realize. The target product can be obtained by the only one-step reaction in the technological process, and the reaction is completed within 2 h. The method avoids resource and energy loss caused by separation of intermediates and tedious operation caused by the step-by-step reaction, reduces time consumption, and greatly improves the synthesis efficiency.