13 results about "Selectfluor" patented technology

The invention relates to a synthesis method of an allyl amine compound. According to the method, 2-methylquinoline or acetophenone derivatives are used as raw materials, a selective fluorine reagent Selectfluor is used as an accelerant, dimethyl sulfoxide and N 'N-dimethylacetamide are used as a mixed solvent, and the allyl amine series compounds are prepared with high yield. The preparation method has the advantages of being low in cost, easy to operate, green, free of pollution and the like, and has potential industrial application prospects. The method provides a green, cheap and convenient way for preparing the allyl amine derivative by using 2-methylquinoline or acetophenone compounds as initiators.

The application discloses a method for constructing fluorine-containing compounds by decarboxylation of alkyl carboxylic acid catalyzed by ketone compounds. The method uses alkyl carboxylic acid with a structure as shown in formula as a reaction raw material, and performs reaction under the joint action of ketone compounds, fluorine-containing reagents and alkali to obtain fluorides shown in formula (1) and formula (2), wherein R 1 are respectively and independently selected from hydrogen, a heterocyclic ring, substituted or unsubstituted aryl, and substituted or unsubstituted hydrocarbyl; R 2 are respectively and independently selected from hydrogen, a heterocyclic ring, substituted or unsubstituted aryl, and substituted or unsubstituted hydrocarbyl; R 3 are respectively and independently selected from hydrogen, a heterocyclic ring, substituted or unsubstituted aryl, and substituted or unsubstituted hydrocarbyl. The reaction method has the advantages of low cost, mild conditions, high reaction efficiency, high yield and high selectivity, and the like. The ketone compounds are used to replace traditional metal catalysts, which can not only provide a fluorine-containing compound library with various structures for candidate drug screening, but also can be applied to positron emission tomography imaging.

The invention belongs to the field of refrigerants, the field of fire fighting, the field of fluorine chemical engineering new materials, the field of foaming agents and the field of chemical synthesis, and particularly relates to a synthesis method of 1, 1, 1, 2, 3-pentafluoropropane and 2, 3, 3, 3-tetrafluoropropene. The synthesis method of the 1, 1, 1, 2, 3-pentafluoropropane comprises the following steps: carrying out a first reaction on 3, 3, 3-trifluoropropene, a first catalyst, an HF source and a selective fluorine reagent in a first solvent to obtain the 1, 1, 1, 2, 3-pentafluoropropane. The synthetic method of the 2, 3, 3, 3-tetrafluoropropene comprises the following step: carrying out a second reaction on the obtained 1, 1, 1, 2, 3-pentafluoropropane in the presence of a second catalyst to obtain the 2, 3, 3, 3-tetrafluoropropene. The synthesis method of 1, 1, 1, 2, 3-pentafluoropropane provided by the invention has the advantages of simplicity in operation, short time consumption, mild reaction, simple reagents required by reaction, high substrate conversion rate, high target product selectivity and the like, and is beneficial to industrial production. The preparation method of 2, 3, 3, 3-tetrafluoropropene provided by the invention has the advantages of safety, environmental protection, simplicity in operation, mild reaction, high yield, high target product selectivity, high reaction speed and the like, and is beneficial to industrial production.

The invention belongs to the field of organic synthesis, and particularly relates to a method for preparing an N, N-difluorobenzenesulfonamide compound under a fluorine-free gas condition. The method comprises the following steps: by taking a benzenesulfonamide compound as an initiator, preparing N-chlorobenzenesulfonamide sodium salt from the benzenesulfonamide compound by using tert-butyl hypochlorite, generating N-fluoro-N-chlorobenzenesulfonamide by using Selectfluor oxidation, and selectively reducing the N-fluoro-N-chlorobenzenesulfonamide into N-fluorobenzenesulfonamide by using sodium borohydride, thereby obtaining the N-fluorobenzenesulfonamide. And finally, carrying out fluorination by using a Selectfluor reagent, so as to generate the target product N, N-difluorobenzenesulfonamide. The method does not need to use highly toxic fluorine gas, the synthesis condition is mild, the separation condition is simple, and the yield is high.

The invention discloses a synthesis method of a benzomorpholone derivative, and belongs to the technical field of organic chemistry. According to the method, a 3-hydroxy-2-indolone derivative and a triazole derivative react in an organic solvent at the temperature of 20-30 DEG C by taking commercialized cheap iodobenzene as a catalyst and selecting a fluorine reagent as an oxidizing agent, so that the benzomorpholone derivative can be obtained. The method is simple to operate, the raw materials are easy to obtain, the reaction steps are short and efficient, and the reaction yield is as high as 96%.

The application discloses a kind of polydifluoroalkylation derivatives of terpene olefin and preparation method thereof, the preparation method includes under inert gas protection, terpene olefin, photosensitizer, cobalt catalyst, organic reducing agent, base, fluorine reagent and organic solvent are sequentially loaded into reaction container, and the reaction system is obtained;Under inert gas protection, the reaction system is reacted at 40~60 ℃ under light condition;After reaction, the system is filtered, rotary evaporated and chromatographically purified, and the polydifluoroalkylation of terpene olefin is completed.The method of the application can efficiently, high selectivity and high yield realize the polydifluoroalkylation reaction of terpene olefin, without using precious metal catalyst, with good functional group compatibility, high yield, and the highest yield can reach 93%.

The invention provides a synthesis method of etifoxacin, and relates to the technical field of organic synthesis, and the synthesis method comprises the following steps: adding triphenylmethyl phosphorus bromide into a solvent, adding potassium tert-butoxide at 0-5 DEG C to obtain a suspension, preparing a 2-aminobenzophenone solution, reacting the suspension at room temperature for 30-40 minutes, adding the 2-aminobenzophenone solution into the suspension, and reacting for 30-40 minutes at room temperature to obtain the etifoxacin. Completely reacting to obtain a compound 2; dissolving the compound 2 in dichloromethane, dropwise adding ethyl isocyanate, heating to room temperature, and reacting to obtain a compound 3; mixing the compound 3, Selectfluor and a compound A, adding acetonitrile, and reacting at room temperature for 60-70 minutes to obtain a compound 4; and reacting the compound 4 and sodium borohydride in ultra-dry dimethyl sulfoxide at room temperature under the protection of nitrogen to obtain etifusin. The compound A is selected from any one of potassium iodide, Selectfluor, tetrabutylammonium chloride and tetrabutylammonium bromide. According to the invention, synthesis of etifusin is realized by a metal-free catalysis and green chemical method, and the yield is high.

The invention belongs to the technical field of trifluoroborate methacrylate production, and particularly relates to a trifluoroborate methacrylate preparation method, which comprises: placing a poor solvent in a reaction container, introducing a boron trifluoride gas, adding methacrylate, filtering, washing, and drying to obtain the trifluoroborate methacrylate. According to the method, boron trifluoride gas is used as a fluorine reagent, so that the problem of water introduction caused by use of a water-containing solvent in a traditional method is avoided, and the product quality and the reaction efficiency are remarkably improved; by using the poor solvent, the yield of the product is improved (greater than or equal to 97%), the method has the characteristics of simplicity in operation and low cost, the generation of three wastes is reduced by fully utilizing the raw materials, and the requirement of large-scale production is met.

The invention belongs to the technical field of battery electrolyte additives, and particularly relates to a preparation method of a lithium fluorophosphate salt, which comprises the following steps: generating a crude liquid lithium salt from an organic lithium salt and phosphorus pentafluoride gas in an organic solvent under low-temperature micro-positive pressure conditions, purifying and crystallizing the crude liquid lithium salt to obtain the lithium fluorophosphate salt, phosphorus pentafluoride gas is used as a fluorine reagent, so that introduction of water is avoided; the micro-positive pressure environment is used, interference of environmental moisture is avoided, the reaction efficiency is improved, one-pot purification and impurity removal are carried out, purification steps are reduced, the production cost is reduced, the method has the advantages of being easy to operate and high in product yield, generation of three wastes is reduced, the method is suitable for large-scale production, the yield of the obtained product can reach 92% or above, and the method is suitable for industrial production. The purity can reach 99% or above.

This invention provides a method and application for adding fluorine at the 9-position of a steroid compound, relating to the field of chemical synthesis technology. The invention uses a compound of formula I as a starting material, reacting it with a first brominating reagent, a second brominating reagent, and hydrochloric acid to undergo a 9,11-position bromohydroxyl reaction to obtain a compound of formula II. Compound II then undergoes a 9-position substitution reaction with a fluorinating reagent to obtain a 9-position fluorinated steroid compound. This invention utilizes mild reaction conditions, avoiding highly toxic and corrosive reagents such as perchloric acid and hydrogen fluoride solution, making it environmentally friendly, with a short reaction route, easy operation, and greater suitability for industrial production.

The invention relates to a synthesis method of an allyl ether compound. According to the method, 2-methylquinoline or acetophenone derivatives are used as raw materials, a selective fluorine reagent Selectfluor is used as an accelerant, dimethyl sulfoxide and ethyl acetate or propyl acetate are used as a mixed solvent, and the allyl ether or propyl ether series derivatives are synthesized with high yield. The preparation method has the advantages of being low in cost, easy to operate, green, free of pollution and the like, and has potential industrial application prospects. The method provides a green, cheap and convenient way for preparing the allyl ether derivative by using 2-methylquinoline or acetophenone compounds as initiators.

The invention provides a defluorination functionalization reaction of beta-trifluoromethyl ketene and a phosphine oxide compound without participation of transition metal. According to the reaction, through a cascade process of three-step selective C (sp3)-F bond cleavage (defluorination phosphorylation, defluorination cyclization and hydrogenation defluorination) of trifluoromethyl, a series of polysubstituted furan derivatives with important synthesis values are modularly synthesized at medium to good yield, and excellent functional group compatibility is shown. The core of the research is to reveal the multiple reaction role of the phosphine oxide compound: the phosphine oxide compound not only serves as a classical phosphorylation reagent, but also serves as a defluorination reagent to break through the activation mode of a traditional P = O compound on an inert C-F bond. It is particularly notable that water is used as a cheap, efficient and environment-friendly proton source in the system and plays a key role in the hydrogenation defluorination step. The method has the advantages of green and mild reaction conditions, good tolerance of functional groups, and high atom economic benefits.

The application relates to the technical field of organic chemistry, and provides a preparation method of aprocitentan or a salt thereof and an intermediate. The application takes a structure shown in formula C or a salt thereof as raw material, carries out a sulfonation reaction with sodium benzenesulfinate to obtain a compound or a salt thereof shown in formula G, carries out a substitution reaction between the compound or the salt thereof shown in formula G and a compound shown in formula B to generate a compound or a salt thereof shown in formula H, and finally carries out a reaction with a sulfonamide to obtain aprocitentan (Aprocitentan) or a salt thereof. The application ingeniously replaces fluorination reagents with cheap and easily obtained sodium benzenesulfinate, utilizes the reactivity of a benzene sulfone group to synthesize Aprocitentan, the raw material is easy to obtain, the cost is lower, the yield is higher, the generated fluorine by-products in the reaction are avoided, the reaction kettle is not corroded by fluorine reagents in industrial production, and the application is particularly suitable for industrial production.