346 results about "Tosylhydrazone" patented technology

The invention provides a method for preparing sludge-based formed magnetic active carbon. The method comprises the steps as follows: sludge is used as a raw material, an activating agent is added for carbonizing and activating the sludge; nano-sized Fe3O4 is used as a magnetic source for magnetizing the sludge active carbon; and sodium carboxymethylcellulose and aluminum salt are composited to an organic-inorganic binding agent, the binding agent and a p-toluenesulfonhydrazide foaming agent are used for uniformly binding powdery magnetic active carbon into a formed magnetic active carbon precursor with abundant pore structures, and finally, the formed magnetic active carbon precursor is heated to obtain the sludge-based formed magnetic active carbon. According to the method, the sludge is used as a main raw material, the resource utilization of the sludge is achieved, the recycling is convenient, and reutilization can be achieved; and further, the sludge-based formed magnetic active carbon has a stable structure and good magnetic stability, and can be widely used in the fields such as sewage treatment, soil pollution treatment and the like.

The invention relates to a synthesis technique of tenofovir, and relates to the field of medicinal chemistry. Using natural (R)-lactate as the starting material, chiral R-1,2-propanediol is obtained through reduction, and then reacted with diethyl carbonate under the action of alkali to obtain the key reaction intermediate R-propylene carbonate ester. Use adenine and R-propylene carbonate to prepare R-9-(2-hydroxypropyl)adenine; Gained R-9-(2-hydroxypropyl)adenine and diethyl p-toluenesulfonyloxyphosphate Under the catalysis of magnesium tert-butoxide, the condensation reaction is carried out to obtain R-9[(diethylphosphorylmethoxy)propyl]purine; the obtained R-9[2-(diethylphosphorylmethoxy) Propyl]purine is hydrolyzed to obtain Tenofovir. The process has short reaction steps, short required reaction time, high quality yield and good product quality, and is suitable for industrialized production.

The present invention relates to a production method capable of producing an optically active α-hydroxyphosphonic acid and its derivatives with sufficiently high enantioselectivity not only for aromatic aldehydes but also for aliphatic aldehydes, and more specifically to a method of producing an optically active α-hydroxyphosphonic acid and its derivatives, characterized in that an optically active aluminum(salalen) complex represented by any one of the following formulae (I), (I′), (II) and (II′):

[wherein R¹s are each alkyl group or aryl group independently; R²s are each alkyl group or aryl group independently; R³s are each alkyl group or aryl group independently, and two R³s may bond with each other to form a ring; R⁴s are each hydrogen atom, halogen atom, alkyl group, alkoxy group, nitro group, or cyano group independently; R⁵ is alkyl group; and X¹ is halogen atom, alkyl group, alkoxy group, acetoxy group or toluenesulfonyloxy group] is used as a catalyst to asymmetrically hydrophosphonylate an aldehyde with phosphonic acid or its derivatives.

The invention discloses a preparation method of capecitabine. The method comprises the following steps: based on D-ribose serving as a starting raw material, carrying out hydroxyl protection, 5-site tosylation, iodine substitution, hypophosphorous acid deiodination and acetylation so as to obtain the key intermediate 12,3-tri-O-acetyl-5-deoxy-beta-D-ribofuranose; carrying out glycosylation on the key intermediate and 5-fluorocytosine; and finally, carrying out N-4 site acylation and deprotection so as to obtain the capecitabine. In the method, a metal catalyst dose not need to be used for participating in reaction, the reaction condition is mild, and the yield is high, thus the method is economical and effective as well as suitable for industrial production on a large scale.

The invention relates to a preparation method of a capillary electro-chromatography column taking beta-cyclodextrin as a bonded stationary phase and an application in a chiral drug separation, and can effectively solve the problems of the capillary electro-chromatography column preparation and the chiral drug separation. The solved technical proposal comprises the following steps: (1) preparing six-bit mono substituted P-toluenesulfonyl-beta-cyclodextrin, (2) preparing six-bit mono substituted ammoniated-beta-cyclodextrin, (3) preparing silylated silica gel, (4) preparing a beta-cyclodextrin bonded silica gel chiral stationary phase, and (5) preparing a capillary packing column. The preparation method is low in cost, low in toxicity and low in environment pollution, and is an innovation of the preparation method of the capillary electro-chromatography column taking the beta-cyclodextrin as the bonded stationary phase and the application in the chiral drug separation.

A method for producing a non-specific adsorption inhibitor includes reacting (A) a tosylated compound of polyoxyethylene monomethyl ether with (B) a polyamine having either an amino group or imino group (—NH—), or both, in total of 3 to 12.

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 invention discloses a new technology for preparing a key intermediate Hoffer's chlorosugar of telbivudine. The technology is characterized in that the technology comprises the following steps: 1, obtaining an epoxide by carrying out condensation, oxidation ring-opening, methylation, tosylation, reduction and epoxidation on vitamin C which is massively supplied in China and is treated as an initial raw material; 2, carrying out ring-opening cyaniding on the obtained epoxide; 3, carrying out sulfuric acid hydrolysis and lactonization on the generated cyan butanetriol derivative; and 4, carrying out hydroxy protection with p-toluoyl chloride, reducing with sodium triacetoxyborohydride to obtain a reduction product, and directly chloridizing the reduction product to obtain the target compound Hoffer's chlorosugar without separation, wherein the Hoffer's chlorosugar is 1-choro-3,5-bis-O-p-toluyl-2-deoxy-L-ribose. According to the technology, the total route yield is 42%, and the product purity is greater than 98%.

The invention relates to an antimicrobial anticorrosive paint and a preparation method thereof. The antimicrobial anticorrosive paint is prepared from the following raw materials in parts by mass: 66-70 parts of acrylic resin, 16-23 parts of castor oil, 10-13 parts of vinyl acetate, 4-6 parts of dimethyl carbonate, 15-18 parts of nano silicon micropowder, 2-7 parts of polyacrylamide, 1-6 parts of 3-aminopropyltriethoxysilane, 1-4 parts of N-ethyl-para-toluene sulfonate, 5-10 parts of zinc oxide, 2-6 parts of bamboo charcoal powder, 90-100 parts of water, 20-30 parts of ethanol and 10-14 parts of ethyl acetate. By reasonably compounding the acrylic resin and other additives, the paint has excellent antimicrobial and anticorrosive properties and excellent adhesiveness. By adding the N-ethyl-para-toluene sulfonate and 3-aminopropyltriethoxysilane, the paint has excellent adhesive force, impact resistance and water resistance.

The invention discloses a compound extender for urea-formaldehyde resin, which is prepared by mixing the following raw materials in parts by weight: 30-40 parts of bean flour, 20-30 parts of wood flour, 10-15 parts of walnut shell flour, 5-10 parts of corn flour, 20-30 parts of modified attapulgite, 10-15 parts of ammonium chloride, 3-6 parts of para toluene sulfonate and 5-10 parts of desugared sodium lignosulfonate. According to the invention, the modified attapulgite contains carboxyl, so that condensation crosslinking with hydroxymethyl of urea-formaldehyde resin is greatly improved, and the dispersion property in the urea-formaldehyde resin is good, thereby reducing the number of hydrophilic groups and improving the water resistance of adhesion. The extender disclosed by the invention is convenient in adhesive mixing method, can reduce or replace extenders such as flour and the like for use and lower the cost, and has high adhesion strength, good shock strength and large elastic modulus. Through chemical bond combination and adsorption of the modified attapulgite, release of free formaldehyde is reduced.

The invention relates to a method for preparing O-tosyl-2-carbamoyl-2-methoxyl-imido-acetamido-oxime, which comprises the following steps: (1) reacting cyanoacetamide, which is used as an initial raw material, with sodium nitrite in a nitrosation mode to obtain a reaction intermediate, and reacting the reaction intermediate with dimethyl sulfate in an esterification mode to obtain 2-cyano-2-methoxyl-imido-acetamide; and (2) under the action of hydroxylamine hydrochloride, hydrolyzing cyano groups in the 2-cyano-2-methoxyl-imido-acetamide obtained in the step (1) into amino groups, and reacting with p-methylbenzene sulfonyl chloride in an esterification mode to generate the O-tosyl-2-carbamoyl-2-methoxyl-imido-acetamido-oxime. The preparation method provided by the invention has the advantages of accessible raw materials, short technical process and high yield, and is suitable for industrial production.

The invention discloses the azido dihydroxypropyl cellulose nitrate preparation method and synthesis which comprises, subjecting natural cotton and cellulose to alkalization under semi-homogeneous phase reaction condition, charging epoxy propyl alcohol for sectionwise etherification to the alkali cellulose, obtaining dihydroxy cellulose ether whose substitution degree is between 0.5-1.2, completely dissolving in dimethyl polyamide / 9% LiCl system, scouring, purifying, drying and dissolving in dimethyl sulfoxide, carrying out homogeneous phase nitrine at high temperature.

The invention discloses a method used for preparing a 4-aminoquinoline derivative. According to the method, an acuprous catalyst, an additive, and o-aminobenzontrile are delivered into a reaction container, wherein the additive is one ingredient selected from triethylamine, tetramethyl ethylenediamine, 1,8-diazabicyclo undec-7-ene, potassium carbonate, or cesium carbonate at will; an organic solvent is added; an alkyne-terminated compound and p-toluenesulfonyl azide are introduced into the reaction container; an obtained mixture is subjected to heating reaction for 3h to 6h at a temperature ranging from room temperature to 100 DEG C, wherein reaction process is monitoring via thin-layer chromatography, and optimal reaction conditions are obtained via selection; after reaction, an obtained mixture is filtered, obtained filter cake is washed, obtained filtrate is mixed, and is subjected to condensation and column chromatography separation so as to obtain the 4-aminoquinoline derivative. One-pot method is adopted to prepare the 4-aminoquinoline derivative, reaction efficiency is increased greatly, post-treatment is simple; and industrialized application prospect is promising.

The invention discloses a method for preparing 7-dehydrogenized cholesteryl ester from 7-tosylhydrazones-3-cholesteryl ester. In an existing method, cholesteryl ester is subjected to esterification, oxidation, hydrazone compounding, hydrazone removing and hydrolyzation to obtain 7-dehydrogenized cholesteryl ester, wherein a hydrazone removing reaction is a typical heterogeneous reaction and is only carried out on the solid surface of an alkali reagent; consequently, the reaction selectivity and the product yield are not high, and thus the production cost is high. The method is characterized in that a crown ether phase transfer catalyst supported by polystyrene resin is adopted for a hydrazone removing reaction. By means of the method, a heterogeneous reaction is converted into a homogeneous reaction, the reaction selectivity is improved, and the conversion rate can be remarkably increased, and the production cost is lower while the product quality is improved. Meanwhile, crown ether obtained after modification and immobilization can be applied repeatedly, and thus the toxicity of common crown ether on the environment is avoided.

The invention discloses an empagliflozin intermediate preparation method, which comprises: carrying out substitution by using p-methoxybenzyl chloride and p-iodoaniline as starting raw materials to obtain a compound IV, performing diazotization and a Sandmeyer reaction to obtain a compound III, further performing demethylation under the action of boron tribromide to obtain a compound II, and finally performing condensation with (S)-3-p-toluenesulfonyloxy tetrahydrofuran to obtain the target compound I, wherein the product purity is greater than or equal to 99.0%. According to the invention, the preparation method has advantages of simple and easily available raw materials, low cost, simple operation steps, simple post-treatment and high product yield, and is suitable for industrial production.

The invention relates to 2-(1,2,4-triazole-1-methyl)-2-(coumarone-5-radical)-1,3-dioxolane with a chemical formula I shown in the description, where R is selected from C1-C2 alkyl radical and C3-C4 linear alkyl radical or branched alkyl radical, R1 selected from H and C1-C2 alkyl radical, X selected from chlorine,bromine,iodine, mesyloxy,trifluoro-mesyloxy, benzenesulfonyl oxy radical, and p-toluenesulfonyl oxy radical, and Y selected from hydrogen, C1-C2 alkoxy, C3-C4 linear alkoxy or branched alkoxy, chlorine, bromine, fluorine or iodine. The chemical formula I is prepared from a key intermediate II of a chemical formula II shown in the description; and a compound I can be applied to preparation of bactericide.

The invention relates to foaming printing ink which comprises the following components in parts by mass: 5-30 parts of para toluene sulfonate, 10-25 parts of azodicarbonamide, 0.1-0.2 parts of defoaming agent, 15-30 parts of ethanol amine, 1-2 parts of cross-linking agent, 50-60 parts of polyvinyl chloride, 60-80 parts of polyvinylidene chloride emulsion, 5-10 parts of epoxy glycol, 0.5-1 part of thickener, 10-20 parts of ethylene glycol, and 1-3 parts of water dispersing pigment. The foaming printing ink is stable to store, nontoxic, odorless, difficult to damage and low in cost, has a three-dimensional effect, improves a decorative art effect, can shorten a technological flow, can lower the printing cost, and can be printed in quantity quickly.

The invention discloses a beta-cyclodextrin derivative and a preparation method and application thereof. The beta-cyclodextrin derivative is a single [6-(2-hydroxy ethyl) amino-6-desoxy]-beta-cyclodextrin, single [6-di(2-hydroxy ethyl) amino-6-desoxy]-beta-cyclodextrin, single [6-(2-hydroxy propyl) amino-6-desoxy]-beta-cyclodextrin, single [ 6 di(2-hydroxy propyl ) amino-6- desoxy]-beta-cyclodextrin, single [6-(3-hydroxy propyl) amino-6-desoxy)-beta-cyclodextrin, single [6-methyl ( 2-hydroxy ethyl ) amino-6-desoxy]-beta-cyclodextrin, single {6- [(2S)-2-hydroxy propyl] amino-6-desoxy}-beta-cyclodextrin and single {6[(2R)-2-hydroxy propyl] amino-6- desoxy}-beta- yclodextrin. The beta-cyclodextrin derivative can be prepared by a nucleophilic substitution reaction of single (6-O-p-toluene sulfonyl)-beta-cyclodextrin and corresponding aminoalcohol. The synthesis method has the advantages of simple operation, mild reaction conditions, simple purification, high yield and good purity of object products. The beta-cyclodextrin derivative can be used as a water-soluble ligand of metal mimic enzyme in aqueous metallic catalytic oxidation and aqueous metallic catalytic reduction reaction.

The invention discloses a method for preparing p-tosyloxymethyl diethyl phosphonate. The method obtains the p-tosyloxymethyl diethyl phosphonate through the following steps: reacting diethyl phosphite and triethylamine with paraformaldehyde at a temperature of 80-110 DEG C, adding an organic solvent after the reaction is completed, cooling to 0-5 DEG C, and adding p-tosylchloride to perform a reaction. The used organic solvent is any one of N,N-dimethyl formamide, tetrahydrofuran, or dioxane, or a mixture mixed by several above solvents with a random mixing ratio. The amount of the organic solvent is 400 g organic solvent per 1 mole p-tosylchloride. The molar ratio of diethyl phosphate, triethylamine, paraformaldehyde and p-tosylchloride is 437:1000:500:500. Paraformaldehyde is added for 2-4 times. The temperature for the reaction performed after p-tosylchloride is added is room temperature, and the reaction time is 10-20 hours. The operation of the method is safe; the product has a correct structure, a high purity, and a high yield; the pollution cost is low; and the method is applicable to industrial production.