1368 results about "P-Toluenesulfonic acid" patented technology

The present invention relates to a new industrial process for the synthesis of solvate- free 17a-acetoxy-11ss-[4-(N,N-dimethyl-amino)-phenyl]-19-norpregna-4,9-diene-3,20-dione [CDB -2914] of formula (I) which is a strong antiprogestogene and antiglucocorticoid agent. The invention also relates to compounds of formula (VII) and (VIII) used as intermediates in the process. The process according to the invention is the following: i) 3-(ethylene-dioxy)-estra-5(10),9(11)-diene-17-one of formula (X) is reacted with potassium acetilyde formed in situ in dry tetrahydrofuran by known method, ii) the obtained 3-(ethylene-dioxy)-17a-ethynyl-17ss-hydroxy-estra-5(10),9(11)-diene of formula (IX) is reacted with phenylsulfenyl chloride in dichloromethane in the presence of triethylamine and acetic acid, iii) the obtained isomeric mixture of 3-(ethylene-dioxy)-21-(phenyl-sulfinyl)-19-norpregna-5(10),9(11),17(20),20-tetraene of formula (VIII) is reacted first with sodium methoxide in methanol, then with trimethyl phosphite, iv) the obtained 3-(ethylene-dioxy)-17a-hydroxy-20-methoxy-19-norpregna-5(10),9(11),20-triene of formula (VII) is reacted with hydrogen chloride in methanol, then v) the obtained 3-(ethylene-dioxy)-17a-hydroxy-19-norpregna-5(10),9(11l); -diene-20- one of formula (VI) is reacted with ethylene glycol hi dichloromethane in the presence of trimethyl orthoformate and p-toluenesulfonic acid by known method, vi) the obtained 3,3,20,20-bis(ethylene-dioxy)-17a-hydroxy-19-norpregna- 5(10),9(11)-diene of formula (V) is reacted with hydrogen peroxide in a mixture of pyridine and dichloromethane in the presence of hexachloroacetone by known method, vii) the obtained 3,3,20,20-bis(ethylene-dioxy)-17a-hydroxy-5,10-epoxy-19-norpregn-9(11)-ene of formula (IV), containing approximately a 1:1 mixture of 5a,10a- and 5ss,10ss-epoxides, is isolated from the solution and reacted with a Grignard reagent obtained from 4-bromo-N,N-dimethyl-aniline in tetrahydrofuran.

The invention discloses a method for preparing a compound of a formula (I) or pharmaceutically acceptable salts thereof. The method is characterized by comprising the following steps of: (1) using a compound of a formula (II) as a raw material and carrying out a reduction and amination reaction with an appropriate reducing agent to obtain a compound of a formula (III); (2) using 2-quinary heterocyclic substituted ethanol as a raw material and reacting to obtain a compound of a formula (IV) under the conditions of appropriate reagent, temperature and solvent; (3) after carrying out chiral separation on the compound of the formula (III), carrying out a condensation reaction with the compound of the formula (I) under an alkaline condition to obtain a compound of a formula (V); and (4) carrying out demethylation protection on the compound of the formula (V) under the condition of appropriate temperature and solvent to obtain the compound of the formula (I), wherein R1 in each formula is selected from C1-8 alkyl groups or aromatic bases which can be arbitrarily substituted, X is selected from halogen atoms or p-toluenesulfonic acid groups and methanesulfonic acid groups for protecting alcoholic extract hydroxyl groups, and Y is selected from O, S and N. A target product obtained by the method has high optical purity, convenient operation, lower cost, higher yield and less pollution and is suitable for industrialized production.

PCT No. PCT/KR96/00250 Sec. 371 Date May 18, 1998 Sec. 102(e) Date May 18, 1998 PCT Filed Dec. 26, 1996 PCT Pub. No. WO97/24358 PCT Pub. Date Jul. 10, 1997The present invention relates to a novel crystalline cefdinir intermediate having formula (II) which can be used very usefully for preparing a cephalosporin antibiotics, cefdinir, in which Ph represents phenyl, p-TsOH represents p-toluenesulfonic acid, and DMAC represents N,N-dimethylacetamide, to a process for preparation thereof and to a process for preparing cefdinir using the compound of formula (II). According to the present invention, cefdinir can be prepared in an excellent color and purity and with a good yield.

The invention discloses a phosphoric-acid-base modified polycarboxylic-acid water reducer with high adaptability and a preparation method thereof. The water reducer is prepared from the following raw materials: isopentenol polyoxyethylene ether, hydrogen peroxide, acrylic acid, an unsaturated phosphoric acid monomer, deionized water, a reducing agent, and a chain transferring agent. The chain transferring agent is one of mercaptoethanol, mercaptoacetic acid and mercaptopropionic acid. The unsaturated phosphoric acid monomer is prepared from 2-phosphono-1,2,4-butanetricarboxylic acid, p-toluenesulfonic acid and hydroquinone. The preparation method for the water reducer comprises adding isopentenol polyoxyethylene ether and deionized water into a reaction vessel, uniformly stirring, heating, keeping warm, adding oxygen peroxide, then dropwise adding a material solution by employing a constant-flow pump, continuing to keep warm for reacting for 1-1.5 h after dropwise adding of the material solution is finished, naturally cooling to room temperature, and adjusting the pH value of the obtained product to 5-6 by using an alkaline solution. The phosphoric-acid-base modified polycarboxylic-acid water reducer possesses good sulfate ion resisting capability and sludge resisting capability, thereby satisfying engineering demand.

The invention discloses a new process for sysnthesizing tenofovir disoproxil fumarate as an antiviral medicament. The invention greatly reforms the preparation process of tenofovir disoproxil as a keyintermediate for synthesizing the tenofovir disoproxil fumarate and establishes a new process suitable for industrial production. The new process includes the following steps: firstly (R)-methyl lactate and diisopropyl-p-ethyl methyl-phosphonate are condensed so that diisopropyl oxygroup- phosphonyl-methyl is introduced and the condensate can be used as a protection group of hydroxyl, and then the reaction step is shortened; secondly, carboxylic ester can be selectively reduced into alcohol by NaBH4 without affecting the phosphonate; and thirdly, adenine and 2-O-( diisopropyl oxygroup- phosphonyl-methyl)-(R)- isopropyl p-toluenesulfonic acid are condensed. Through hydrolysis, the enofovir disoproxil (II) as the key intermediate can be conveniently obtained, and the optical purity can reach more than 98%.

The invention relates to a near infrared BODIPY fluorescence dye and a preparation method thereof. A BODIPY derivative and 2-aldotruxene undergo a Knoevenagel condensation reaction under the catalysis action of p-toluenesulfonic acid and piperidine to synthesize the dye, and the maximal absorption wavelength and the maximal emission wavelength of the dye in an organic solvent are 650nm or above respectively. The preparation method has the advantages of simple reaction steps, mild reaction conditions and good selectivity. Like fluorescence dyes have the advantages of high molar extinction coefficient, good solubility and light stability, excellent photophysical performances, and good application prospect in cell imaging and biological marking.

The invention provides a novel synthesis method for pimavanserin. The method comprises the steps that a compound formula (1a) is adopted as a raw material for preparing an active urea compound formula (1) and then subjected to a reaction with a compound formula (2) under an alkaline system to obtain a pimavanserin free alkali formula (3), and then pimavanserin free alkali forms a salt with tartaric acid to obtain a pimavanserin half tartrate formula (4). The method is simple in technological path, low in cost and suitable for industrial production. The formula is shown in the description, wherein HmA is the general formula of m-basic acid, HnA is the general formula of n-basic acid, m and n are 1 or 2 or 3, and the m-basic acid and the n-basic acid are selected from sulfuric acid, hydrochloric acid, phosphoric acid, p-toluenesulfonic acid, benzenesulfonic acid, methanesulfonic acid, methanoic acid, acetic acid, trifluoroacetic acid, oxalic acid, citric acid or tartaric acid.

The invention discloses a making method of 3.4.3'.4'-biphenyl tetracarboxylic dianhydride, which comprises the following steps: adopting 4-chlorophthalandione anhydride as raw material; preparing 4-chlorophthalandione dimethyl ester, 3.3'.4.4'-biphenyl tetracarboxylic tetramethyl ester, 3.3'.4.4'-biphenyl tetracarboxylic acid and 3.3'.4.4'-biphenyl tetracarboxylic dianhydride; coupling; hydrolyzing; refining; (1) adopting p-toluenesulfonic acid as esterifying catalyst in the preparing procedure of 4-chlorophthalandione dimethyl ester; (2) adopting acetonitrile as solvent in the coupling procedure; (3) purifying hydrolytic 3.3'.4.4'-biphenyl tetracarboxylic acid through deionized water in the refining procedure; (4) washing and purifying 3.3'.4.4'-biphenyl tetracarboxylic dianhydride through acetone.

The disclosed preparation method for acetylized glucal comprises: preparing the D-acetylized glucose catalyzed by acids (HClO4, H2SO4, ZnCl2, AlCl3, p-toluenesulfonic acid and methanesulfonic acid); without separation or purification, leading directly the product into HBr or equivalent (such as PBr3 and water) to obtain and then recrystallize the coarse 1-bromoacetyl glucose with one of ethyl ether, propyl ether and isopropyl ether; adding Zn, ZnCl2, methanol and Co-ion catalyst to prepare the coarse target; recrystallizing with alcohol for the refined product. This invention saves step and reduces cost.

The invention belongs to the technical field of coatings, and discloses polyurethane-amino resin modified waterborne alkyd resin and preparation and application thereof. The resin is prepared from, by mass, 23.8-31.5 parts of vegetable oil, 10-14.6 parts of polyhydric alcohol, 10-17.3 parts of polyatomic acid, 0.03-0.05 part of alcoholysis catalyst, 24-30.4 parts of diisocyanate, 0.03-0.09 part of dibutyltin dilaurate, 1-4 parts of 1,4-butanediol, 3-7 parts of 2,2-dihydromethyl propionic acid, 1.6-8 parts of amino resin, 0.25-1.25 parts of p-toluenesulfonic acid, 2-6 parts of neutralizer and 1.2-1.9 parts of micromolecular chain extender. The vegetable oil is used as the raw material, and the amino resin is introduced through chemical modification, so that the obtained waterborne alkyd resin is low in cost, the hardness, water resistance, solvent resistance, heat resistance and tensile strength of a resin paint film are improved, and the application prospects are good.

The invention relates to a preparation method of topiroxostat, which comprises the following steps: reacting an initial raw material compound isoniazide disclosed as Formula (6) with a compound 4-cyano-pyridyl-N-oxide disclosed as Formula (5) to generate a triazole compound disclosed as Formula (4), reacting the triazole compound disclosed as Formula (4) in the presence of a copper catalyst (CuX), zinc cyanide (Zn(CN)2) and dimethylamino formyl chloride to generate a cyanotriazole compound disclosed as Formula (3), reacting the compound disclosed as Formula (3) in the presence of p-toluenesulfonic acid to generate a compound disclosed as Formula (2), and finally, alkalifying with inorganic alkali to obtain the target compound disclosed as Formula (1) (topiroxostat). The method is simple in operation and after-treatment, and greatly lowers the consumption of the zinc cyanide due to the use of the copper catalyst, so that the reaction conditions are milder, and the purity of the prepared product is high; and the method is suitable for industrial production.

The invention relates to a paint remover for plane aluminium alloy skin depainting treatment; the paint remover comprises more than two kinds of 70-80 parts of main solvent, two kinds of 12-18 parts of accelerators, 4-5 parts of thickening agents and 0.5-2 parts of corrosion inhibitors; the main solvent includes N-methylpyrrolidone (N-P), alpha-pyrrolidone (alpha-P), benzyl alcohol and dimethyl sulfoxide; the accelerator is soluble organic acid with lower than 1000 of molecular weight, and the molecular weight includes methanoic acid, salicylic acid, p-toluenesulfonic acid and terephthalic acid; the thickening agent is carboxymethylcellulose or carboxyethyl cellulose; and the corrosion inhibitor is p-methyl pyrrodiazole, thiazole and benzotriazole. The paint remover can remove the paint film on the surface of the plane aluminium alloy skin in a short time (within 35min) in a in-situ way, and the paint remover has no over etching to the surface of the aluminium alloy and has recoatability.

A semiconductor wafer cleaning formulation for use in post plasma ashing semiconductor fabrication comprising at least one organic chelating agent and at least one polar solvent, wherein the chelating agent and polar solvent are in sufficient amounts to effectively remove inorganic compound residue from a semiconductor wafer. Preferably, the chelating agent is selected from the group consisting of 2,4-Pentanedione, Malonic acid, Oxalic acid, p-Toluenesulfonic acid, and Trifluoroacetic acid; and the polar solvent is selected from the group consisting of Water, Ethylene glycol, N-Methylpyrrolidone (NMP), Gamma butyrolactone (BLO), Cyclohexylpyrrolidone (CHP), Sulfolane, 1,4-Butanediol, and Butyl carbitol.

The invention belongs to the technical field of functional materials, and mainly relates to a method for preparing a shell-core magnetic composite resin microsphere adsorbent with lignin-modified phenolic resin under an acid condition. The method includes the following steps: magnetic ferroferric oxide particles and lignin phenolic resin are first prepared, the ferroferric oxide particles and the lignin phenolic resin are uniformly mixed according to a certain proportion, a certain amount of reversed-phase solvent and surfactant is added, uniform stirring is sufficiently carried out, p-toluenesulfonic acid solution is then added, acid curing is carried out under certain temperature and stirring speed, and thereby magnetic microspheres are formed. The invention adopts an organic acid with weak acidity as acid curing agent and creatively adopts an acid low-temperature curing method to prepare the composite microspheres with uniform size by means of a reversed-phase suspension method. The microspheres have magnetism and the adsorption property of lignin, and can serve as an adsorbent to adsorb colored matters and heavy metal ions in wastewater, moreover, an additional magnet can be utilized to rapidly carry out the separation of water and the microspheres, and thereby a convenient and efficient separation method is provided for wastewater treatment.

The invention relates to an esterification and termination synthesis method of allyl polyether, which comprises the steps of taking allyl polyether and acetic acid as raw materials, and carrying out esterification in a reactor under the action of a catalyst and a dehydrating agent, wherein the molar mixing ratio of the allyl polyether to the acetic acid is 1: 1.0-3.0; the catalyst is p-toluenesulfonic acid, and the using quantity by weight thereof accounts for 0.1-2.0% of the total weight of fed materials; and the dehydrating agent is toluene, and the using quantity by weight thereof accounts for 20-50% of the total weight of the fed materials. The esterification and termination synthesis method of the allyl polyether has the advantages of simple and easy operation, low cost and high termination ratio, thereby being applicable to the large-scale industrial production of the esterified terminated allyl polyether.

The invention discloses a synthesizing method of N-phenyl maleimide, which comprises the following steps: 1) acylating the maleic anhydride and aniline in the solvent; 2) reacting N-phenyl maleamic acid with hydroquinone as inhibitor and p-toluenesulfonic acid and N-ethyl pyrrolidone as double catalyst; decompressing the liquid to remove solvent; obtaining the rought product; 3) recrystallizing to obtain the product.

The invention discloses a preparation method of ceftizole sodium, which belongs to the field of medicinal chemistry. The method uses 1H-tetrazolium acetic acid and 2-mercapto-1,3,4-thiadiazole as raw materials, and generates 1H-tetrazolium acetic acid-1 under the catalysis of p-toluenesulfonic acid or dicyclohexylcarbodiimide ,3,4-thiadiazole-2-thioester (active ester), and then the active ester and 7-aminocephalosporanic acid are "one-pot" synthesis of ceftizole acid under the action of quaternary ammonium salt phase transfer catalyst, and then Sodium salt is generated, and further recrystallization and purification can obtain high-purity ceftiazole sodium. The preparation process is simple and feasible, the atom utilization rate is high, the product quality is good, and the industrial production requirements are met.

The invention relates to a near-infrared truxene-based conjugate dual-BODIPY fluorescent dye and a preparation method thereof. The fluorescent dye is synthesized by virtue of Knoevenagel condensation reaction of a BODIPY derivative and dialdehyde-containing truxene under the catalysis of p-toluenesulfonic acid and piperidine. The preparation method has the beneficial effects of simple reaction steps, mild reaction conditions and relatively good selectivity. The fluorescent dye has excellent physical properties of relatively high molar extinction coefficients, good solubility and light stability and the like, the highest electronic absorption spectrum red shift reaches above 650nm, the fluorescence emission wavelength reaches 680nm, and the fluorescent dye has very high application prospects. The fluorescent dye has good potential application prospects in the fields of cell imaging, bio-labeling or photoelectric materials and the like.

An etchant includes: 5 to 20 wt % of persulfate, 1 to 10 wt % of at least one compound of an inorganic acid, an inorganic acid salt, or a mixture thereof, 0.3 to 5 wt % of a cyclic amine compound, 1 to 10 wt % of at least one compound of an organic acid, an organic acid salt, or a mixture thereof, 0.1 to 5 wt % of p-toluenesulfonic acid, and water, based on the total weight of the etchant. A copper-titanium etchant further includes 0.01 to 2 wt % of a fluoride-containing compound. A method of forming a display device using the etchant, and a display device, are also disclosed.

The invention relates to an ONS (Organometallics) type salicylaldimine binuclear metallic alkene catalyst as well as a preparation method thereof and the application thereof. Under an effect of p-toluenesulfonic acid, bisalicylaldehyde or a bisalicylaldehyde derivative performs condensation reaction with amines containing sulfur atoms in an alcohol solution so as to obtain Schiff base; and the obtained Schiff base has complexing reaction with IVB group transition metal under water-free and oxygen-free conditions so as to obtain the ONS type salicylaldimine binuclear metallic alkene catalyst. Compared with a mononuclear metal alkene catalyst, the ONS type salicylaldimine binuclear metallic alkene catalyst provided by the invention has the advantages of higher catalytic activity and better thermal stability due to binuclear metallic synergistic effect during catalyzing ethylene homopolymerisation or ethylene and 1-hexene copolymerization. Under the pressure of a methylaluminoxane (MAO) or triethylaluminium assisted catalyst and 1 atm ethylene, the ethylene homopolymerisation is catalyzed and the activity can reach 1.6*10<6> gPE/molTi.h; and during catalyzing the ethylene and 1-hexene copolymerization, the activity reaches 3.8*10<5> gPE/molTi.h.

The invention relates to a phthalaznone-containing poly(aryl ether nitrile) end-capped with maleimide and a preparation method thereof. Self-made 4-[4-(4-carboxyl phenoxyl) phenyl) -2-(4-carboxyl phenyl) naphthyridine-1-ketone or derivative thereof and 2, 6-dichlorobenzonitrile are used as polycondensation monomers. Meanwhile, other bisphenol and aromatic bi-halogen monomers can be added, p-aminophenol is used as an end-capping agent, and a solvent, a co-boiling dewatering agent and a catalyst are added for carrying out progressive polymerization reaction and synthesizing a phthalaznone-containing poly(aryl ether nitrile) resin end-capped with amino. On the basis, a phthalaznone-containing poly(aryl ether nitrile) polymer end-capped with amino, maleic anhydride, p-toluenesulfonic acid, a polymerization inhibitor, the solvent and the co-boiling dewatering agent are used as raw materials to prepare a phthalaznone-containing poly(aryl ether nitrile) resin end-capped with maleimide. The poly(aryl ether nitrile) resin can be co-cured with bis-maleimide or an epoxy resin, can be used in the fields of thermostable paint, coatings, adhesives, composite materials and the like and has broad application prospects.