61 results about "Nitroethylene" patented technology

The invention belongs to the field of medicine synthesis, and in particular relates to a preparation method of a Rucaparib intermediate 6-fluoro-3-[(E)-2-nitroethylene]-1H-indole-4-methyl formate. 3-amino-5-methyl fluorobenzoate is used as a raw material in the method, which reacts with a zinc reagent of 2-(2-bromoethyl)-1,3-dioxolane after being diazotized, then is hydrolyzed, and reacts with nitromethane. The preparation method has cheap and easily available materials, a refined reaction route, high reaction selectivity and high yield.

The invention discloses difluoroethyl-containing nitrosamine compounds and a preparation method thereof. A series of difluoroethyl-containing nitrosamine derivatives are obtained by taking carboxylicacid as a catalyst and carrying out an aza-Michael addition/nitrosation tandem reaction on three components, i.e., difluoroethylamine, tert-butyl nitrite and 1-aryl 2-nitroethylene at room temperaturein absence of other organic solvents. Molecular skeletons of the compounds contain potentially bioactive difluoroethyl and nitrosamine groups, thus establishing a material basis for drug discovery and druggability evaluation, and having an important application value. The preparation method provided by the invention adopts the easy-to-obtain raw materials, does not need an additional organic solvent, and has the advantages of mild reaction conditions, simple operation, high yield and good substrate universality.

The invention discloses a method for synthesizing 4-aryl-4,5-dihydrofuran under the catalysis of alkali, In the method aryl substituted nitroethylene and a 1,3-dicarbonyl compound taken as raw materials and dimethylsulfoxide taken as a solvent are reacted for 0.5 to 8 hours at the temperature of between 30 and 80 DEG C under the catalysis of the alkali to directly obtain the 4-aryl-4,5-dihydrofuran by a one pot method.

The invention discloses a new chemical synthesizing method of 1-motol-1-methylmercapto-2-nitroethylene as one intermediate of ulcer drug ranitidine, which comprises the following steps: adopting nitromethane, carbon bisulphide and potassium hydroxide as initial reacting material; synthesizing 1, 1-dimethyldisulphide-2-nitro ethylene to dissolve in the water; reacting with aminomethane to synthesize new intermediate product; filtering to obtain the product.

The invention discloses a preparation technology for a 3-aryl-4-nitro isoxazole compound. The preparation technology comprises the following steps: synthesizing a compound shown as formula II through the nucleophilic addition of hydroxylamine hydrochloride and the compound shown as formula I used as the raw material; acquiring the compound shown as formula III through the substitution reaction of the compound shown as formula II and N-chlorosuccinimide; preparing 1-dimethyl amino-2-nitro ethylene through the reaction of N,N-dimethylformamide dimethyl acetal and nitromethane used as the raw material; and acquiring a target product 3-aryl-4-nitro isoxazole compound through the cyclization reaction of the compound shown as formula III and 1-dimethyl amino-2-nitro ethylene. The raw materials in the synthesis route are low in cost and easily acquired, the operation condition is mild and is easily controlled, the product is easily purified and the preparation technology is a new method for synthesizing the 3-aryl-4-nitro isoxazole compound.

A sugar ester derivative of the general formula (I) wherein G stands for a group of the formula (A) or a group of the formula (B) wherein lambda means 0 or 1; at least one of R1 and R2 means an ester residue of a saturated or unsaturated fatty acid having 1-30 carbon atoms and the other group means hydrogen atom or acetyl group, and R3 means a group of the formula (C) wherein X means a halogen atom, m means an integer of 0 to 4, Y means hydroxy group, an alkoxy group, a carboxyl group or sulfonic acid group, n means 0 or 1 and Z means nitro group or nitrovinyl group and its use. The sugar ester derivative of the general formula (I) is useful as a substrate for the measurement of lipase or esterase activities, and the reagents and the methods for measuring lipase or esterase activities which comprise said sugar ester derivative as the substrate are excellent in terms of reproducibility and sensitivity and enable the measurement of lipase or esterase activities in accordance with rate-assay method by an easy procedure.

The invention relates to a method for synthesizing 2-thienyl ethylamine by means of biological catalysis. The method comprises the steps of preparing glucose, disodium hydrogen phosphate and potassium dihydrogen phosphate into a water solution according to a certain proportion, sterilizing and cooling to obtain a bacillus licheniformis culture medium; activating the obtained bacillus licheniformis culture medium in a shaking table at the constant temperature according to a certain cell concentration; then, dissolving 2-nitro vinyl thiophene, adding the solution into the activated culture medium, carrying out a biological catalysis reaction, and then carrying out centrifugal separation; extracting supernatant by using ethyl acetate, washing, drying, and carrying out reduced pressure distillation to obtain the product 2-thienyl ethylamine. The method has the remarkable characteristics and progress of being simple in technology, high in synthetic yield, low in cost and less in environmental pollution.

The invention relates to a synthesis method of 2-nitroethenyl thiophene. The synthesis method comprises the following steps: adding 2-thiophenecarboxaldehyde, nitromethane, beta-alanine dissolved with acetonitrile and a solvent into a reaction flask, reacting for 1h under unltrasound irradiation; after reaction, removing acetonitrile, filtering out beta-alanine, concentrating, and recrystallizing residues to obtain 2-nitroethenyl thiophene. The synthesis method provided by the invention has the characteristics of low cost, simpleness and convenience in operation, high yield and the like, and is suitable for industrial production.

The invention relates to a preparation method of 1-amino-1-hydrazino-2,2-dinitroethylene bismuth salt. The method comprises the following steps: synthetizing 1-amino-1-hydrazino-2,2-dinitroethylene potassium salt by using 1,1-diamino-2,2-dinitroethylene, hydrazine hydrate and KOH as raw materials, then reacting with soluble metal salts such as bismuth nitrate to prepare 1-amino-1-hydrazino-2,2-dinitroethylene bismuth salt. The synthesis method is simple; the industrialized production is easy to operate; and the synthesized 1-amino-1-hydrazino-2,2-dinitroethylene bismuth salt is a new high-energy compound, is used as green and energetic combustion catalyst and can be used to greatly reduce the burning rate pressure exponents of the double-base propellant and the modified double-base propellant.

The invention discloses a preparation method of nitenpyram. The method comprises the steps: carrying out a catalytic reaction in a low-grade chlorinated hydrocarbon solvent by taking N-ethyl-2-chloro-5-pyridinemethylamine and 1,1-dichloro-2-nitroethylene as starting raw materials and anion exchange resin as an acid binding catalyst, ending the reaction, and carrying out filtration to remove the anion exchange resin to obtain a solution of an intermediate compound (II); introducing methylamine gases to the solution of the intermediate compound (II), ending the reaction, and carrying out filtration; and concentrating a filtrate, and separating out a crystal to obtain a target compound (I). The invention provides the preparation method of a synthesis process of nitenpyram, the preparation method is few in reaction steps, simple in process as well as green and environment-friendly in process, and nitenpyram is high in yield and quality. Compared with an existing technical process, the preparation method is simple and convenient in process operation, low in operation cost, free of wastewater discharge, capable of realizing recycle of the catalyst, green and environment-friendly in process, high in product quality and yield, low in cost, very suitable for industrial production and extremely high in industrial application value.

The invention discloses a method for preparing spherical 1,1-diamino-2,2-dinitroethylene crystals by ultrasonic assistance, and the method comprises the following steps of: 1) adding Fox-7, an organicsolvent and an additive into a crystallization kettle to be fully dissolved to prepare a saturated solution, wherein the water temperature of the crystallization kettle is controlled at 20-40 DEG C;(2) adding an antisolvent dropwise to the saturated solution while stirring to form a supersaturated solution and then performing crystal nuclei generating and crystal growth; 3) after the crystal iscompletely separated out, performing ultrasonic treatment on the crystal in mother liquor while stirring, wherein the ultrasonic treatment time is 1-3 hours, and the ultrasonic frequency is 30-70 khz;and 4) filtering, washing and drying to obtain a spherical FOX-7 crystal. The spherical FOX-7 crystal prepared by the method has smooth surface, few transparent defects in the crystal and good fluidity; the process is simple and easy to control, the anti-solvent consumption is small and recyclable, the reaction conditions are mild, safe and reliable, green and efficient, and industrialization iseasy to realize.

A method for preparing (E)-1, 3-diphenyl-4-nitro-1-butene comprises the following steps: using (E)-1-dimethylamino-2-nitroethylene (I), (E)-1, 3-diphenyl propylene (II) as raw materials, using 1, 2-dichloroethane as a solvent, reacting at room temperature to be complete under the combined action of DDQ and an acidic catalyst, and then carrying out post-treatment on the reaction solution to obtaina target product (III); the method has the advantages of high yield, simple and safe operation, easily obtained raw materials and the like.

The invention relates to the field of fructose-1,6-biphosphatase inhibitors, and specifically discloses a nitroethylene-containing ester compound. The ester compound is the compound as shown in a formula (1). The invention further discloses a preparation method of the compound as shown in the formula (1). The invention further discloses another nitroethylene-containing ester compound which is the compound as shown in the formula (2). The invention further discloses a preparation method of the compound as shown in the formula (2). The invention further provides application of the nitroethylene-containing ester compounds or pharmaceutically acceptable salt in preparation of medicines such as the medicine for inhibiting fructose-1,6-biphosphatase, and the medicine for treating or preventing gluconeogenesis metabolic disease or thrombus diseases.

The invention discloses a method for synthesizing 2-amino-5-nitrothiazole, which comprises the following steps: (1) in an inert atmosphere, adding diethylamine, acetyl chloride and triethyl orthoacetate into a reaction container, uniformly mixing, stirring to react for 12-24 hours, and distilling and purifying the reaction product to obtain N, N-dimethylformamide dimethyl acetal, (2) in an inert atmosphere, mixing N, N-dimethylformamide dimethyl acetal with nitromethane, heating the mixture to 80-100 DEG C for reflux reaction, carrying out reduced pressure distillation on the reaction productto remove the solvent, and purifying to obtain N, N-dimethyl nitroethylene, and (3) in an inert atmosphere, putting N, N-dimethyl nitroethylene into a reaction container, sequentially adding ethanol,liquid bromine and thiourea, reacting at room temperature, after the reaction is finished, filtering a reactant, washing with ice ethanol, drying to obtain a white solid, adding water, and filtering to obtain the 2-amino-5-nitrothiazole. According to the method for synthesizing 2-amino-5-nitrothiazole, the raw materials are easy to obtain, the cost is low, and the yield can reach 60%.

The invention discloses a 3-4'-5-trihydroxystilbene nitroethylene compound as well as a preparation method and application thereof, and relates to the technical field of drug design and synthesis. The3-4'-5-trihydroxystilbene nitroethylene compound has the following general formula (the formula is shown in the description). According to the 3-4'-5-trihydroxystilbene nitroethylene compound as wellas the preparation method and application thereof, the 3-4'-5-trihydroxystilbene nitroethylene compound is designed and prepared, and the prepared 3-4'-5-trihydroxystilbene nitroethylene compound isapplied to the preparation of anti-cancer drugs; the results of biological activity tests show that the 3-4'-5-trihydroxystilbene nitroethylene compound has good inhibiting activity on a human gastriccancer cell line MGC 803, a human liver cancer cell line SMMC-7721 and a human breast cancer cell line MDA-MB-231, and thus, the preparation of the 3-4'-5-trihydroxystilbene nitroethylene compound isof great significance for screening out novel anti-cancer drugs.

The invention provides a 1, 1-diamino-2, 2-dinitroethylene/nano aluminum powder composite energetic particle as well as a preparation method and application thereof, and relates to the technical field of explosives. The 1, 1-diamino-2, 2-dinitroethylene/nano aluminum powder composite energetic particle provided by the invention is of a core-shell structure and comprises nano aluminum powder, and 1, 1-diamino-2, 2-dinitroethylene and an adhesive which are coated on the surface of the nano aluminum powder. According to the composite energetic particle provided by the invention, the nano aluminum powder is taken as a core, the 1, 1-diamino-2, 2-dinitroethylene and the adhesive are taken as a shell, and the 1, 1-diamino-2, 2-dinitroethylene, the adhesive and the nano aluminum powder are tightly combined to form a uniform coating structure, so that the spontaneous agglomeration of the nano aluminum powder can be effectively inhibited; the problem of non-uniform component distribution of the nano aluminum-containing explosive is solved, and the heat and mass transfer distance among the components is reduced, so that the energy release rate of the detonation reaction of the explosive and the reaction completeness of the nano aluminum powder are enhanced.

The invention discloses a preparation method of 5-hydroxytryptamine hydrochloride, and particularly relates to a method for efficiently synthesizing the 5-hydroxytryptamine hydrochloride by taking 5-hydroxyindole and nitroethylene as raw materials through addition reaction and reduction reaction. The preparation method of the 5-hydroxytryptamine hydrochloride provided by the invention is a preparation method which is high in yield, low in cost, less in three wastes, good in product purity and suitable for industrialization.

The invention relates to a preparation method of water-soluble cationic polyamidine, which comprises the following steps that S1, in an organic solvent, dinitrovinyl benzene, N, N-dibromocarbamate and bis-secondary amine react to prepare t-butyloxycarbonyl substituted polyamidine, the reaction temperature is 40-80 DEG C, and the reaction time is 6-72 hours; the molar ratio of the dinitrovinyl benzene to the N, N-dibromocarbamate to the bis-secondary amine is 1: 2: (0.5-2), and the concentration of the dinitrovinyl benzene is 0.01-10 mol/L; and S2, the t-butyloxycarboryl is removed to obtain the water-soluble cationic polyamidine. The water-soluble cationic polyamidine is prepared by using dinitrovinyl benzene, N, N-dibromocarbamate and bis-secondary amine as raw materials through reaction, the preparation method is simple to operate, mild in reaction condition, environment-friendly and free of a metal catalyst, the prepared water-soluble cationic polyamidine has water solubility, the biocompatibility is improved, and the gene can be effectively entrapped.

A method for synthesizing 1-methyl amino-1-methoxy-2-nitroethylene relates to a compound. The invention provides a method of high yield coefficient and purity quotient for synthesizing 1-methyl amino-1-methoxy-2-nitroethylene, the method is applicable to large-scale industrial production. A catalyst is dissolved in absolute methanol solution; 1-methyl amino-1-methyl mercapto-2-nitroethylene are added in, stirred and heated up to reflow; the methyl alcohol is processed by reduced pressure evaporation to dryness to obtain a yellow solid matter; and the solid matter obtained by recrystalization by ethyl alcohol is the target product. The invention does not need to use methylene dichloride highly toxic solvent, thereby having advantages in production operation safety and environmental protection. The used raw materials are low in cost and available, unit operations are less, the steps like extraction and dryness, and the like, are saved, the operation safety of operating personnel is improved, the unit operation production period is shortened, and the production cost is greatly reduced, thus being suitable for industrial production. The yield coefficient of the reaction can be increased from 35.2% to 40-65%, thus obviously reducing the cost.