50 results about "Sodium trifluoromethanesulfinate" patented technology

The invention relates to an application of a biomass-supported copper-catalyzed three-component reaction in preparation of a fluorine-containing medicine, which comprises the following steps: catalyzing quinoxalinone and derivatives thereof, indole and derivatives thereof and sodium trifluoromethanesulfinate by using a copper catalyst taking chitosan as a carrier, so as to synthesize the 3-(2-(trifluoromethyl)-indol-3-yl) quinoxalin-2-one derivative from the three components by a one-pot method. The heterogeneous biomass copper-loaded catalyst is adopted to catalyze the reaction, and the problems that a traditional homogeneous catalyst cannot be recycled, and metal residues exist are solved; and the 3-(2-(trifluoromethyl)-indol-3-yl)quinoxalin-2-one compound with different substituent groups is expanded, the biomass supported copper catalyst can be cyclically catalyzed for multiple times, the target product keeps good yield, and it is indicated that the catalyst has efficient cycle capacity and can promote the possibility of industrialization of a reaction system.

The invention discloses a synthesis process of high-quality sodium trifluoromethanesulfinate. The synthesis process comprises the following steps: A, mixing sodium hydrosulfite with trifluoromethyl bromide and sodium hydroxide, adding the mixture into a reaction kettle, and heating to react to obtain a mixed solution of sodium trifluoromethanesulfinate and sodium bromide; B, feeding the mixed solution obtained in the step A into a layering kettle, and standing for layering to obtain a supernatant and a lower filtrate; C, extracting supernatant, adding the lower filtrate into a stirring kettle,and adding an extracting agent into the stirring kettle for extraction reaction under stirring; D, feeding the reaction product in the processing step C into a desolventizing kettle for desolventizing to obtain a semi-finished product; and E, finally, drying the semi-finished product through a high-speed centrifugal spray dryer to obtain sodium trifluoromethanesulfinate. The synthesis process issimple in operation, pollution-free in synthesis process, high in purity of sodium trifluoromethanesulfinate, high in yield, capable of effectively reducing production cost, capable of saving energy and reducing consumption and good in economic benefit.

The present invention provides a method for producing various types of arylbis(perfluoroalkylsulfonyl)methane having a bulky aryl group and an electron-accepting aryl group in which synthesis was conventionally considered to be difficult, at high efficiency; a novel arylbis(perfluoroalkylsulfonyl)methane that can be widely applied to asymmertric catalyst, various types of functional materials and the like; and a metallic salt thereof. In addition, excellent catalysts are also provided. An aryl halomethane is reacted with a sodium trifluoromethane sulfinate, the arylmethyl triflone produced thereby is reacted with a t-BuLi and the like, the lithium salt of the arylmethyl triflone obtained is reacted with a trifluoromethane sulfonic acid anhydride, and an arylbis(trifluoromethylsulfony)methane such as pentafluorophenylbis(triflyl)methane, {4-(pentafluorophenyl)-2,3,5,6-tetrafluorophenyl}bis(triflyl)methane and the like are obtained at a high yield.

The invention discloses a method for preparing a trifluoro-methylmercapto-substituted indole compound. The method comprises the following step: by taking trifluoro-methyl sodium sulfonate as a trifluoro-methylmercapto source and triphenylphosphine as a reducing agent, under the action of a visible light catalyst eosin Y, and enabling a substituted indole compound, the trifluoro-methyl sodium sulfonate and triphenylphosphine to react with N-chloro-o-phthalimide, thereby obtaining the trifluoro-methylmercapto-substituted indole compound. The method disclosed by the invention is simple, a trifluoro-methylmercapto reagent used in the method is low in toxicity, and no heating is needed in the preparation process, so that the energy can be saved, the environment can be protected, and direct trifluoro-methylmercapto reaction of a 3-position C (sp2)-H bond of an indole compound is achieved.

The invention provides a preparation process of trifluoromethyl sulfinyl chloride. The preparation process comprises the steps as follows: 1) a synthesis kettle is taken, and thionyl chloride is added; 2) thionyl chloride is heated until reflux and cooled to 0-5 DEG C, and sodium trifluoromethanesulfinate is fed; 3) the temperature is increased to 15-20 DEG C, distillation is performed, the steam is turned off and the temperature is reduced to 10 DEG C or lower when the temperature reaches 90-100 DEG C, and water is added to clean a distillation kettle; 4) the material is distilled into a rectifying still, the rectifying still starts to heat up, front cut fractions are collected after reflux for 3-5 hours, whether the material in the reflux pipe is transparent is observed when the temperature reaches 40-45 DEG C, and a finished product of trifluoromethyl sulfinyl chloride is collected if the material is transparent, and reflux is continued if the material is not transparent; 5) the finished product is stopped from being collected when the temperature reaches 45-50 DEG C, reflux is continued, and the finished product of trifluoromethyl sulfinyl chloride continues to be collected after the reflux temperature is reduced. The process is simple to operate, is green and has no pollutant discharge during preparation, is energy-saving, consumption-reducing and good in economic benefit, an adopted solvent is recyclable, obtained trifluoromethyl sulfinyl chloride has high purity and yield, and the production cost can be effectively reduced.

The invention discloses a method for converting benzene into benzotrifluoride through heterogeneous catalysis. Benzene is catalyzed to generate benzotrifluoride at lower temperature and normal pressure with manganese sulfate monohydrate as a catalyst, sodium trifluoromethanesulfinate as a trifluoromethyl source and acetonitrile as solvent. The raw materials are low in price and easy to obtain, conditions are mild, environment pollution is low, products are easy to separate, hydrogen fluoride, sulfur tetrafluoride and other highly-corrosive and highly-toxic fluorinated reagents used in current industrial trifluoromethylation reactions are avoided, large-scale industrial production is facilitated, and the method can be further used for trifluoromethyl modification of organic compounds with biological activity and medicine activity and has good application prospects and economic benefits.

The invention provides a kind of allyl salicylaldehyde (I) compound as the starting material for the reaction, sodium trifluoromethyl sulfinate (II) as the trifluoromethyl source and persulfate as the oxidant, The trifluoromethyl-containing chroman-4-one target compound (III) and its preparation method. The method involves mild reaction conditions, simple operation, product diversity, and can realize gram-scale production.