22 results about "Selectfluor" patented technology

The invention belongs to the technical field of fine chemical engineering, and particularly discloses a method for preparing a broad-spectrum bactericide 2-n-butylbenzo [d] isothiazole-3 (2H)-ketone by a molecular editing method. The preparation method comprises the following specific steps: taking 3H-1, 2-benzodisulfophenol-3-ketone and n-butylamine as raw materials, taking Selectfluor as an additive, adding the raw materials and the additive into a mixed solvent, and carrying out heating and stirring reaction, so as to obtain the target product 2-n-butylbenzo [d] isothiazole-3 (2H)-ketone (BBIT). The method is simple and convenient to operate, the raw materials are easy to obtain, the yield is high, thiophenol raw materials or excessive alkali are prevented from being used, and potential application value is achieved.

The invention discloses a preparation method of fluorohydrocortisone acetate, and belongs to the technical field of medicine synthesis. According to the method, the fluorine hydrocortisone acetate is obtained through one-step reaction by taking the Anecortisone acetate as an initial raw material and taking a mixture of an organic solvent and water as a solvent under the condition of a Fe (III) reagent and a fluorine reagent. The preparation method disclosed by the invention is simple and convenient to operate, high in safety, mild in reaction condition, low in cost, high in yield, small in corrosivity and suitable for industrial mass production; meanwhile, the problems that in the prior art, operation is inconvenient, corrosivity is high, toxicity is large, dangerousness is high, the requirement for equipment is high, and the yield is low are solved, and a new technical scheme more suitable for industrial production is provided.

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 application provides a preparation method and a packaging method of isoflurane, and belongs to the technical field of halogen-containing acyclic compounds. Trifluoroethanol and difluoro-chloromethane are used as starting materials, a selective fluorine reagent and NaCl solid are added, and the trifluoroethanol and the difluoro-chloromethane are etherified. Under the action of the selective fluorine reagent, the obtained etherification intermediate is chlorinated with NaCl, the reaction temperature of etherification and chlorination is 60-120 DEG C, and one-pot isoflurane preparation without intermediate taking is carried out. The preparation method has simple steps, simple subsequent treatment, and can obtain a product with high purity.

The patent relates to a method for preparing marine terpenoid natural products based on a decarboxylation coupling reaction of carboxylic acid salt of sclareolide or carboxylic acid of sclareolide and quinone compounds, and belongs to the field of chemical synthesis. The method takes sclareolide as raw material, and realizes, for the first time, a Minisci decarboxylation coupling reaction of carboxylic acid salt of bicyclic sesquiterpene or carboxylic acid of sclareolide and p-benzoquinone promoted by Selectfluor, so that the synthesis steps of yahazunone are shortened from the previous 6-18 steps to 2 steps, and asymmetric synthesis of multiple yahazunone natural products is realized. The method has the characteristics of good step economy, simple operation and suitability for industrial production.

The invention provides a preparation method of a 9-fluorinated steroid compound, which comprises the following steps: a compound I reacts with a fluorination reagent to obtain a 9-fluorinated steroid compound II, the reaction formula is as follows: in the formula I and the formula II, R1 and R2 are respectively and independently selected from hydrogen, hydroxyl or hydroxyl with a protecting group, and the 16-position carbon is R configuration or S configuration and represents a single bond or a double bond; the fluorination reagent is selected from Selectfluor or Selectfluor II, and the fluorination reagent is selected from Selectfluor I and Selectfluor II. According to the preparation method of the 9-fluorinated steroid compound II, the 9-fluorinated steroid compound II is prepared by taking a steroid compound as a raw material through a one-step reaction, after the reaction is completed, a fluorination reagent in a reaction solution is quenched, water is added into the reaction solution, and a solid is separated out by cooling and stirring, so that a target product can be obtained. The preparation method provided by the invention has few steps, does not need to use strong corrosive acid, is simple to operate and is suitable for industrial large-scale production.

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 application discloses a preparation method of octafluorocyclopentene, and reaction is carried out in two steps. First, 4-cyclopentene-1,3-dione is reacted with a selective fluorine reagent under reflux in acetonitrile to generate a crude product, a second mixture, the second mixture is purified and then is put into a second step reaction, and is reacted with diethylamine sulfide in dichloromethane to generate a third mixture. The reaction process is environment-friendly and simple, basically no three wastes are generated, is cheap and easy to obtain, the reaction process is simple and mild, nitrogen protection is needed and no waste gas pollution is generated, the method is easy to operate, and is suitable for industrial production.

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 multi-(hetero) aromatic hydrocarbon substance carbon-fluorine bond hydrogenation defluorination reaction with HP (O) Ph2 as a defluorination reagent and H2O as an environment-friendly accelerant under a metal-free condition. The method is mild in reaction condition and good in functional group tolerance, has the characteristics of simple post-treatment, green steps, low pollution, high economic benefits and the like, can smoothly realize carbon-fluorine bond hydrogenation defluorination of multi-(hetero) aromatic hydrocarbon substances containing complex molecules, and is expected to promote green and sustainable defluorination chemical development.

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.

The invention discloses a synthesis method of a nitrogen-fluorine reagent mediated sulfur-fluorine compound, which comprises the following steps: by taking sulfenamide as a raw material and a cheap and easily available nitrogen-fluorine reagent as a fluorine source, adding a proper amount of alkali, and carrying out one-step reaction to synthesize sulfimide acyl fluoride and sulfodiimine fluorine compounds. According to the method, sulfenamide is subjected to one-step oxidation and fluorination to generate sulfimide acyl fluoride and sulfodiimine fluorine, the raw materials are easy to obtain, the reaction condition is mild, the reaction time is short, the substrate range is wide, post-treatment is simple and convenient, no catalyst is needed, and the popularization and application prospects are wide.

The invention discloses a synthesis method of sulfonamide compounds, which comprises the following steps: mixing a sulfonamide compound containing an S-N structure, a selective fluorine reagent and water, and stirring at room temperature to realize selective oxidation of sulfonamide so as to obtain a series of sulfonamide compounds. According to the method, the synthesis of the sulfinamide compound can be efficiently realized, additional additives are not needed in the reaction, the reaction cost is reduced, the reaction is carried out in a water phase, no organic solvent is needed, and the green chemistry concept is met. The synthesis reaction operation is simple, the conditions are mild, the reaction is fast, the yield is high, the post-treatment is convenient, the amplification of the reaction can be realized, and the method has wide application prospect and practical value.