70 results about "Ethoxybenzene" patented technology

The invention relates to 1-[3-(6, 7-dihydro-1-methyl-7-oxo-3-propyl-1H-pyrazol parallel [4, 3-d] pyridine-5-thyl)-4-ethoxybenzene sulfonyl]-cis-3, 5-lupetazin citrate or citric acid alidenafil crystalform A and preparation method thereof and also relates to drug combination containing citric acid alidenafil crystal form A and application thereof in preparation of drug for treating erection disturbance. Citric acid alidenafil raw material is dissolved with distilled water in certain proportion, stirring is carried out for 60-80 minutes while temperature is maintained to be 38-42 DEG C, and stirring is carried out for 10-15 hours while temperature is maintained to be 20-26 DEG C, thus obtaining the product. Test by an X-ray powder diffractometer, thermogravimetric analysis and infrared spectrometer proves that an unprecedented citric acid alidenafil crystal form A is obtained, the crystal form A can form a combination with one or multiple pharmaceutically acceptable carrier, excipient or diluent and can be effectively applied to treatment on andropathy.

The invention relates to 1-[3-(6, 7-dihydro-1-methyl-7-oxo-3-propyl-1H-pyrazole parallel [4, 3-d] pyridine-5-thyl)-4-ethoxylbenzene sulfonyl]-cis-3, 5-lupetazin citrate or citric acid alidenafil crystal form D and preparation method thereof and also relates to drug combination containing citric acid alidenafil crystal form D and application thereof in preparation of drug for treating erection disturbance. Citric acid alidenafil raw material is dissolved in distilled water/acetone mixed solution in certain proportion, and heat preservation is carried out for 50-72 hours while stirring is carried out at certain temperature, thus obtaining the product. Test by an X-ray powder diffractometer, thermogravimetric analysis and infrared spectrometer proves that an unprecedented citric acid alidenafil crystal form D is obtained, the crystal form D can form a combination with one or multiple pharmaceutically acceptable carrier, excipient or diluent and can be effectively applied to treatment on andropathy.

The invention relates to a preparation method of o-ethoxybenzoic acid, which comprises the following steps: adding salicylic acid, acetone and potassium hydroxide into a reaction bulb, dropwisely adding bromoethane while stirring at room temperature, heating under reflux for 9-15 hours, recovering the acetone under reduced pressure, adding water and liquid alkali, heating under reflux for 2-4 hours, cooling to room temperature, regulating the pH value to 3-4 with glacial acetic acid, cooling to 1-15 DEG C, separating by vacuum filtration, washing with water, and carrying out vacuum drying to obtain the o-ethoxybenzoic acid, wherein the salicylic acid:potassium hydroxide:bromoethane:liquid alkali mol ratio is 1:(2.0-2.5):(2.1-2.5):1.4. The method has the advantages of simple technique, low raw material cost, high yield and good quality, and is convenient to operate and convenient for industrial production.

This invention relates to a method for synthesizing vardenafil hydrochloride. The method comprises: (1) performing acylation and nucleophilic addition on D,L-alanine raw material, condensing with 2-ethoxybenzamidine hydrochloride twice, and performing ring-closing reaction to obtain 2-(2-ethoxyphenyl)-5-methyl-7-propyl-3H-imidazo[5,1-f][1,2,4]-trizin-4-one; (2) performing sulfonation reaction to obtain 4-ethoxy-3-(3,4-dihydroxy-5-methyl-4-oxo-7-propyl imidazo[1,5-f][1,2,4]trizin-4-one)benzenesulfonic acid; (3) reacting with N-ethyl pyrazine to obtain vardenafil, and reacting with HCl to obtain vardenafil hydrochloride. The method has such advantages as easy operation, high yield, and simple process and low reaction condition requirement, thus is suitable for industrialization.

A calcium or a magnesium salt of (2S)-2-ethoxy-3-(4-{2[hexyl(2-phenylethyl)amino]-2-oxoethoxy}phenyl)propanoic acid.

The invention relates to 1-[3-(6,7-dihydro-1-methyl-7-oxo-3-propyl-1H-pyrazolo [4,3-d] pyrimidine-5-yl)-4-ethoxybenzenesulfonyl]-cis-3,5-dimethyl-piperazine citrate or a aildenafil citrate crystal form C and a preparation method thereof. The invention also relates to a medicinal composition containing the aildenafil citrate crystal form C and application thereof in preparing medicaments for treating male erection disturbance. An unprecedented aildenafil citrate crystal form C is proved to be obtained through the steps of dissolving an aildenafil citrate raw material in a mixed solution of distilled water and acetone at a certain proportion, keeping the temperature for 8 to 10 hours at a certain temperature while stirring, and testing the prepared product by an X-ray powder diffractometer, a thermogravimetric analyzer and an infrared spectrometer; and the crystal form C can form a composition together with one or more pharmaceutically acceptable carriers, an excipient or a diluent, and can be effectively applied to the treatment of andropathy.

The invention discloses a preparation method and an application of fluorine-containing microspheres without stabilizers on the surfaces. Anhydrous THF (tetrahydrofuran) is added to a single-neck flask, mPEG (methoxy polyethylene glycol), an RAFT reagent CEPDB (4-(2-carboxyethylcarbonyl)oxy-ethoxy phenyl dithiocarbamate isobutyronitrile ester) and DMAP (4-dimethylaminopyridine) are dissolved in anhydrous THF, the single-neck flask is placed in an ice-water bath, and the mixture is stirred and cooled to 0 DEG C; DCC (dicyclohexylcarbodiimide) is dissolved in anhydrous THF, and a DCC-THF solution is obtained; the DCC-THF solution is all dropwise added to the single-neck flask within 30-50 min, and the single-neck flask is continuously placed in the ice-water bath for a reaction for 1 h after the DCC-THF solution is dropwise added. The method is rapid, environment-friendly and energy-saving, and fluorine-containing polymer microspheres without stabilizers on the surfaces are rapidly prepared with an optical RAFT dispersion polymerization method and a thermal aftertreatment method with an ethanol/water mixed solvent as a reaction medium. The preparation method is simple and the reaction speed is high.

A cell culture apparatus and a method for fabricating the cell culture apparatus are disclosed, the method comprises forming at least one fillister on a biomaterial composite layer by photolithography, wherein the biomaterial composite layer contains two gel materials. One is a bio-compatible hydrogel composition having various weight ratio of: 2-hydroxyethylmathacrylate (HEMA), bisphenol A and glycidyl methacrylate (bis-GMA), triethylene glycol dimethacrylate (TEGDMA), r-methacryloxypropyl trimethoxysilane (MAPTMS), α,α-diethoxyacetophenone (DEAP), and the other one is a photo-sensitive silica gel composition.

The invention provides a preparation method for a nanocapsule. The preparation method is characterized by comprising the following steps: (1) subjecting water, surfactant, cosurfactant and an oil phase to a stirring reaction at 10 to 80 DEG C for 2 min to 5 h so as to obtain a stable transparent microemulsion; (2) adding ethyl orthosilicate and ammonia water, carrying out a hydrolysis reaction for 0.1 to 12 h, then adding N-isopropyl acrylamide, polyacrylic acid and a photoinitiator diethoxyacetophenone and carrying out a reaction for 0.1 to 12 h so as to obtain micro-nano spheres; (3) subjecting the micro-nano spheres to ultraviolet irradiation so as to initiate polymerization of function groups; and (4) removing silica particles so as to obtain the nanocapsule. Compared with the prior art, the invention has the following advantages: since a reversed-phase microemulsion process is employed to prepare a template, the nanocapsule has a small particle size; and poly(N-isopropyl acrylamide) and polyacrylic acid are used as capsule wall materials, so double responsiveness to a pH value and temperature is obtained.

The invention relates to a synthetic method of a 2,2-diethoxy acetophenone photoinitiator, which comprises the following steps: a, synthesizing ethyl nitrite, namely mixing ethanol with 28 percent of aqueous solution of sodium nitrite in a reaction kettle with mechanical stirring and a gas ingress pipe, dripping 20 percent dilute sulphuric acid into the mixture at the temperature of between 20 and 30 DEG C to generate ethyl nitrite gas, and directing introducing the generate ethyl nitrite gas into the step b for reaction, wherein the molar ratio of the ethanol to the sodium nitrite to the dilute sulphuric acid is 1.00:1.09 to 1.68:1.10 to 1.18; and b, synthesizing 2,2-diethoxy acetophenone, namely introducing the ethyl nitrite gas generated by the step a into acetophenone and 36 percent hydrogen chloride ethanol solution, and neutralizing the mixture by using sodium hydroxide solution after a reaction ends to prepare finished products, wherein the molar ratio of the acetophenone to the hydrogen chloride ethanol solution is 1:1. The synthetic method is simple and convenient in process and high in product yield and is suitable for industrial production.

The invention provides a preparation method of 2-(4-oxethyl phenyl)-2-methyl propanol. The preparation method comprises the following steps of (1) dissolving 2-(4-oxethyl phenyl)-2-methyl ethyl propanoate in an ethyl alcohol solvent, and adding potassium borohydrate and lithium chloride; after ending reaction, dropwise adding hydrochloric acid, adding water, recovering the solvent under reduced pressure, extracting by using dichloromethane, drying an organic phase by using sodium sulphate anhydrous, and carrying out vacuum concentration, thus obtaining the 2-(4-oxethyl phenyl)-2-methyl propanol. The preparation method has the advantages that the dangerousness is reduced, and the process is relatively reasonable, simple and convenient. The 2-(4-oxethyl phenyl)-2-methyl propanol is low in cost, high in quality, environment-friendly and is suitable for industrial production. The reaction total yield can reach above 80% by the 2-(4-oxethyl phenyl)-2-methyl ethyl propanoate, and the content of the product reaches 98%.

The invention relates to a method for synthesizing o-ethoxybenzoic acid from salicylic acid and acetone, which comprises the following steps: adding salicylic acid, acetone and potassium hydroxide into a reaction bulb, dropwisely adding bromoethane while stirring at room temperature, heating under reflux for 9-15 hours, recovering the acetone under reduced pressure, adding water and liquid alkali, heating under reflux for 2-4 hours, cooling to room temperature, regulating the pH value to 3-4 with glacial acetic acid, cooling to 1-15 DEG C, separating by vacuum filtration, washing with water, and carrying out vacuum drying to obtain the o-ethoxybenzoic acid, wherein the salicylic acid:potassium hydroxide:bromoethane:liquid alkali mol ratio is 1:(2.0-2.5):(2.1-2.5):1.3. The method has the advantages of simple technique, low raw material cost, high yield and good quality, and is convenient to operate and convenient for industrial production.

The invention discloses a preparation method of 3-bromophenyl azide1-(3-azidopropyl)-3-bromo-4-ethoxybenzene. 3-(3-bromo-4-ethoxyphenyl)acrylic acid is used as a starting material, a target product 5 is obtained through reduction, hydrogenation, Ms (methylsulfonyl) loading and azidation reactions, and the product is used as a template micro-molecule for synthesis of various compound libraries.

The o-ethoxyl phenol refining process includes the following steps: alkali washing condensated o-ethoxyl phenol oil phase or o-ethoxyl phenol product obtained through catechol process with 5-20 % sodium hydroxide solution for 30 min and separating liquid; regulating pH value of the water phase after alkali washing with hydrochloric acid to 1-4, extracting with toluene, and separating liquid to collect oil phase; distilling the oil phase at 110-120 deg.c to recover toluene, lowering the temperature to 30-40 deg.c for decompression rectification to obtain o-ethoxyl phenol of purity not lower than 99.2 %, with the recovered toluene being reused. The present invention can raise the production capacity of industrial apparatus and lower production cost.

The invention provides a method for preparing 4-ethoxy phenylacetic acid, and the method comprises the following steps of: (1), reacting phenetole with dimethyl formamide under the catalysis of phosphorus oxychloride to prepare 4-ethoxy benzaldehyde; (2), reacting the 4-ethoxy benzaldehyde with chloroform under the action of a phase transfer catalyst to prepare 4-ethoxy-alpha-hydroxyphenylacetic acid; and (3), carrying out a hydrogenolysis reaction on the 4-ethoxy-alpha-hydroxyphenylacetic acid in the presence of a reducing agent to prepare the 4-ethoxy phenylacetic acid. By using the synthetic route of the method, the final 4-ethoxy phenylacetic acid is prepared through aromatic formolatiom, phase transfer catalysis and a reduction reaction; compared with a preparation procedure using the chloromethylation of the phenetole and the cyanidation of sodium cyanide in the prior art, side products are less; the purification of a product is easier; the pollution is small; in addition, as the sodium cyanide is not needed, numerous requirements on safety production and post treatment do not exist; a process is easy to achieve; and the safety is high.