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338 results about "Tosyl chloride" patented technology

Synthesis process of vecuronium bromide

The invention discloses a synthesis process of vecuronium bromide. The synthesis process comprises the following steps: generating epiandrosterone sulfonyl ester (III) by carrying out esterification reaction between epiandrosterone (II) and paratoluensulfonylchloride; generating 5Alpha-androst-2-alkene-17-ketone (IV) by carrying out elimination and dehydration reaction between the (III) and 2,6-lutidines; generating 17-acetoxyl-5Alpha-androstane-2,16-diene (V) by carrying out enolization and esterification reaction between the (IV) and isopropenyl acetate; generating (2Alpha, 3Alpha, 16Alpha,17Alpha)-diepoxy-17Beta-acetyl-5Alpha-androstane (VI) by epoxy reaction of the (V) under the effect of hydrogen peroxide; generating 2Beta, 16Beta-di(1-piperidyl)-5Alpha-androstane-3Alpha-hydroxyl-17-ketone (VII) by ring-opening and addition reaction of the (VI) under the effect of hexahydropyridine; generating 2Beta, 16Beta-di(1-piperidyl)-5Alpha-androstane-3Alpha,17Beta-diol (VIII) by the (VII)under the reduction of potassium borohydride; generating 2Beta, 16Beta-di(1-piperidyl)-3Alpha, 17Beta- acetoxyl-5Alpha-androstane (IX) by carrying out esterification reaction of the (VIII) under the acetylation of acetic anhydride; and generating vecuronium bromide (I) by carrying out quaternary ammonium salt reaction between the (IX) and bromomethane. The invention has the advantages of low cost,less pollution and high yield.
Owner:XUZHOU NORMAL UNIVERSITY

Method for synthesizing mometasone furoate or monohydrate of mometasone furoate

ActiveCN106279340AThe generation of solutionNo generationSteroidsAfter treatmentMometasone furoate monohydrate
The invention belongs to a synthesizing method for medicine, and particularly relates to a method for synthesizing mometasone furoate or a monohydrate of the mometasone furoate. The method includes the steps that 8-DM serving as a first compound is used as an initial material, and the first compound and paratoluensulfonyl chloride are subjected to a sulfonylation reaction to generate a second compound; the second compound is not subjected to after-treatment and is subjected to a chlorination reaction with RCl (R is Li, Na, K and Et3N) to generate a third compound; the third compound is not subjected to after-treatment, a part of organic alkali is replenished, and the mixture and furoyl chloride are subjected to an esterification reaction to generate a fourth compound; the fourth compound is not subjected to after-treatment, acid adjustment is carried out, a large quantity of chlorine elements existing in a reaction system are used for a ring-opening reaction, and the mometasone furoate or the mometasone-furoate monohydrate is obtained. The method is simple in technology, mild in reaction condition, high in yield, low in cost, high in quality and raw-auxiliary-material using rate, free of genetic toxicity impurity generation and suitable for industrial production.
Owner:山东锐顺药业有限公司

Preparation method of methyl p-tolyl sulfone

The invention relates to a preparation method of methyl p-tolyl sulfone, which belongs to the technical field of sulphone preparation, in particular to a preparation method of the methyl p-tolyl sulfone by taking monochloro methane as a methylating agent for synthesis. The preparation method is characterized by taking p-toluenesulfonylchloride, anhydrous sodium sulfite, sodium bicarbonate and monochloro methane as synthesizing raw materials and comprising the following operation steps: a. salifying the p-toluenesulfonylchloride; b. synthesizing the methyl p-tolyl sulfone; c. adjusting pH, reducing the temperature and discharging; d. filtering, dehydrating and drying; and e. inspecting the quality and packaging and warehousing after qualification. The invention provides a preparation methodof the methyl p-tolyl sulfone without using a deadly poisonous compound of dimethyl sulfate as a raw material, and has safe operation, environmental protection, short production period, good productquality, high yield, low production cost and strong market competitiveness. The content of the methyl p-tolyl sulfone reaches up to 99.5 percent, and the yield of the methyl p-tolyl sulfone, which iscounted by the p-toluenesulfonylchloride of the raw material, is more than or equal to 85 percent.
Owner:SHANDONG XINGHUI CHEM

Side chain, synthesis method thereof, and method for synthesizing hydroxychloroquine sulfate from side chain

The invention discloses a side chain, a synthesis method thereof, and a method for synthesizing hydroxychloroquine sulfate from the side chain. The synthesis method of the side chain comprises the following steps: 1, condensing N-ethylethanolamine and 5-chloro-2-pentanone to obtain a condensation product; 2, esterifying the condensation product and an acetyl reagent to obtain an esterification product; 3, reducing the esterification product to obtain a reduction product; and 4, reacting the reduction product with a halogenating agent to obtain the side chain. The synthesis method of the hydroxychloroquine sulfate comprises the following steps: 1, reacting 4-amino-7-chloroquinoline with paratoluensulfonyl chloride to obtain 4-Tos-amino-7-chloroquinoline; 2, reacting the side chain with the 4-Tos-amino-7-chloroquinoline to obtain a hydroxyquine base; and 3, reacting the hydroxyquine base with sulfuric acid to obtain the hydroxychloroquine sulfate. The synthesis method of the new side chain avoids the ammonification process and the catalytic hydrogenation process, and is safe and environmentally friendly, and the hydroxychloroquine sulfate can be obtained through low-temperature condensation of the side chain, so the quality of the above products is remarkably improved, and the production flow is simplified.
Owner:宜宾莱特医药化工有限公司

Preparation method of tiamulin base

InactiveCN102675172AHarm reductionReduce salt formation and crystallization stepsSulfide preparationReaction temperatureKetone
The invention relates to a preparation method of tiamulin base. The preparation method includes: filtering pleuromulin fermentation broth, drying mycelium, performing leaching by using methanol as solvent, using acetone to extract leach liquor after vacuum concentration, concentrating extract, transferring concentrate into a synthetic reactor, adding paratoluensulfonyl chloride, allowing for synthetic reaction at pH of 11-12 and reaction temperature of 20-30 DEG C, allowing for standing and layering after complete reaction, adding tetrabutylammonium bromide and diethylaminoethyl mercaptide into ketone phase respectively , allowing for full reaction at pH of 9-10 and the reaction temperature of 50-60 DEG C, adding water for extraction, discarding aqueous phase, filtering the ketone phase, and reducing the original volume to 60-70% by vacuum concentration to obtain tiamulin base. The original process is improved, the salifying and crystallization process is omitted, the tiamulin base is used to produce preparations directly, and accordingly equipment investment cost and production cost are lowered, product quality is improved, and the content of tiamulin base reaches 80-90%. Organic solvents used in the preparation method are recyclable, environmental pollution is reduced, and the preparation method has promising development prospect.
Owner:宁夏泰瑞制药股份有限公司

Thiophene polycyclic organic semiconductor material synthesis based on pyrene

The invention discloses thiophene polycyclic organic semiconductor material synthesis based on pyrene and belongs to the field of photoelectric conversion materials. The molecular formulas of compounds are C<76>H<86>N<4>S<4> and C<62>H<80>N<2>S<2>, and the structural formula can be seen in the Application of the invention. A synthesis method comprises the steps of making the pyrene react with liquid bromine, and obtaining 1,3,6,8-tetrabromo pyrene; making the 1,3,6,8-tetrabromo pyrene react with 1-octyne, obtaining a product, and then using palladium/carbon for conducting catalytic reaction,and obtaining 1,3,6,8-quadri-octane pyrene; using ruthenium trichloride for catalyzing the 1,3,6,8-quadri-octane pyrene, adjusting the using amount of sodium periodate, and obtaining tetrone and diketone; then making o-phenylenediamine and sulfoxide chloride react with liquid bromine, and obtaining 4,7-dibromo-2,1,3-diazosulfide; making thiophene react with thiadiazole, and obtaining diazosulfide; then making o-phenylenediamine and paratoluensulfonyl chloride react with liquid bromine, subsequently, making the mixture react with concentrated sulfuric acid, then making the mixture react with thionyl chloride, and obtaining 5,6-dibromo-2,1,3-diazosulfide; conducting operation same with the reaction process, and obtaining another type of diazosulfide; making a thiadiazole product to be subjected to ring-opening reaction, and obtaining two types of o-phenylenediamine products; making the tetrone and the diketone react with the two types of o-phenylenediamine respectively, and obtaining the compounds.
Owner:BEIJING INSTITUTE OF TECHNOLOGYGY
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