37 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 relates to a preparation method of lithium fluoroborate containing unsaturated bonds, and belongs to the technical field of lithium ion battery additives. The preparation method comprises the following steps: carrying out reaction on organic acid lithium containing unsaturated bonds and boron trifluoride gas in a solvent at a low temperature of-10 to 0 DEG C, and carrying out solid-liquid separation to obtain a lithium fluoroborate crude product containing unsaturated bonds; the solvent is a poor solvent of lithium fluoroborate containing unsaturated bonds. According to the method, boron trifluoride gas is used as a fluorine reagent, so that introduction of water is avoided; the method has the advantages of simple operation, high product quality, high yield, low cost, full utilization of raw materials, reduction of the generation of three wastes, and suitableness for large-scale production. The yield of the obtained product can reach 96% or above, and the purity can reach 99% or above.

The invention discloses a preparation method of octafluorocyclopentene, which comprises the following two steps of: firstly, reacting 4-cyclopentene-1, 3-diketone with a selective fluorine reagent in acetonitrile under the condition of reflux to generate a crude product second mixture, purifying the second mixture, and putting the purified second mixture into a second-step reaction to obtain the octafluorocyclopentene. Reacting with diethylamino sulfur trifluoride in dichloromethane to generate a third mixture; the method has the advantages of environment-friendly and simple reaction process, no generation of three wastes, low cost, easy obtaining, simple reaction process, mild reaction, no generation of waste gas pollution even if nitrogen protection is needed, easy operation, and suitableness for industrial production.

The invention relates to a preparation method of 3, 5-difluoropiperidine and derivatives thereof, which comprises the following steps: in an organic solvent, under the catalysis of an organic primary amine catalyst, enabling piperidone raw materials of different protection types as shown in a formula (I) to react with an electrophilic fluorination reagent to generate a compound as shown in a formula (II), and further reducing to generate a compound as shown in a formula (III). According to the method, a piperidone compound is taken as a raw material, and an electrophilic fluorination reagent such as N-fluorobenzenesulfonamide (NFSI) or a SelectFluor reagent is taken as a fluorine source, so that the 3, 5-difluoropiperidine and the derivative thereof are prepared. The method is simple to operate, mild in reaction condition and easy in reaction purification. In addition, by adjusting the catalyst, the method can also be used for preparing a corresponding optically pure multi-chiral center product.

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 present invention discloses a class of alkyl zinc reagents and a preparation method and application thereof, belonging to the technical field of synthetic organic chemistry. The general structural formula of the alkyl zinc reagent of the present invention is: R‑znOPiv·Mg(OPiv)Br, wherein R is selected from a chain alkyl, a cyclic alkyl or a substituted alkyl. The present invention completes the preparation of a Grignard reagent by lithium salt catalysis or iodine element catalysis, and then completes the preparation of a zinc reagent by transmetallation and an inorganic salt activation strategy to synthesize an alkyl-substituted alkyl difluoro reagent, and the general structural formula of the alkyl-substituted alkyl difluoro reagent is: #imgabs0# wherein R1 is selected from an ester group, an alkyl group, an alkynyl group, an amide, a benzoxazole, diethyl phosphate or a perfluoro-substituted alkyl group; R is selected from a chain alkyl group, a cyclic alkyl group or a substituted alkyl group; R2, R3 are independently selected from a substituted alkyl group; and R4 is selected from an ester group. The alkyl zinc reagent is applied to the bifunctional reaction of olefins, and the alkyl-substituted alkyl difluoro reagent is applied in click chemistry reactions.

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 chiral 3-hydroxy-4-fluoropiperidine derivative and a synthesis method thereof.The synthesis method comprises the steps that a compound N-tert-butyloxycarbonyl-4-piperidone serves as an initial raw material, carbonyl of a tetrahydropyrrole compound is activated firstly, then the tetrahydropyrrole compound reacts with nitrosobenzene, and a chiral nitrogen oxide compound is generated; and then denitrifying in sulfate to generate alpha-hydroxy ketone. Then carbonyl is reduced by a reducing agent to generate an ortho-dihydroxy compound, the ortho-dihydroxy compound is attacked by a selective fluorine reagent to obtain a chiral hydroxyl-fluorine compound, and the chiral hydroxyl-fluorine compound is resolved by a resolving agent to obtain a target product. The synthetic method has the advantages of short steps, low cost and simplicity and convenience in operation, is suitable for large-scale industrial production, and can be used as a drug intermediate or used for researching potential drugs.

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 present invention relates to a method for catalytically hydrating carbonylation of arylacetylene by using the photothermal effect of gold nanoparticles, belonging to the technical field of catalysts. This method uses a photochemical synthesis method, with a xenon lamp as the light source, gold particles (AuNPs) as the photothermal material, tetrabutylammonium bromide and the selective fluorine reagent Selectfluor as additives, and under the action of Al, the hydration carbonylation of aryl alkynes is realized. When the reaction proceeds for 5 h, the separation yield of the carbonyl product is as high as 90.5%. This method uses photocatalysis to efficiently realize the carbonylation of alkynes under mild conditions without acid and strong oxidants.

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 present invention provides a method for preparing unprotected β-amino fluoride by iron-catalyzed olefin ammonia fluorination reaction, belonging to the technical field of compound preparation method. The method is to use olefin and oxidative amination reagent as reaction substrates, fluorine reagent as nucleophilic fluorine source, divalent iron salt Fe (II) as catalyst, react in air to obtain unprotected β-amino fluoride. This method uses olefin as reaction substrate, introduces nitrogen atom and fluorine atom simultaneously by one-step reaction, greatly shortens the synthesis step of β-amino fluoride, improves preparation efficiency, and shortens time.

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 invention discloses a preparation method of N-((phenylamino) carbonyl) sulfamoyl fluoride, and belongs to the field of organic chemical synthesis. According to the method, in a specific dichloromethane solvent, an aniline compound and an isocyanate compound react under the action of a fluorine reagent to obtain the N-((phenylamino) carbonyl) sulfamoyl fluoride compound. According to the method, cheap and easily available antimony trifluoride is adopted as a fluorine source, the substrate applicability is wide, the raw materials are simple and easily available, the economic cost is low, and the target product can be efficiently obtained.

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 discloses a preparation method of an organic diazide compound, and belongs to the technical field of organic synthesis. The preparation method comprises the following steps: in a reaction system without metal participation, trimethylsilyl azide is used as an azide source, a selective fluorine reagent is used as an activating agent, a carbon-nitrogen bond is constructed, the selective fluorine reagent promotes a substrate compound and trimethylsilyl azide to be subjected to a diazido reaction in acetonitrile in a nitrogen atmosphere, purification is performed after the reaction is completed, and the trimethylsilyl azide is obtained. A product compound is obtained. According to the preparation method of the organic diazide compound, a series of diazide products are synthesized with high separation yield (the highest separation yield can reach 93%), and the method is easy to operate, mild in reaction condition, good in reaction system tolerance and capable of tolerating various substrates.

The invention relates to the technical field of organic synthesis, in particular to a method for preparing a compound simultaneously containing a benzisothiazolinone skeleton and a benzothiazine-4-ketone skeleton. Derivatives containing a benzisothiazolinone skeleton and a benzothiazine-4-ketone skeleton at the same time have not been reported yet. In order to solve the problems, the invention provides the method for preparing the compound simultaneously containing the benzisothiazolinone skeleton and the benzothiazine-4-one skeleton, 1, 2-benzisothiazolin-3-one and Selectfluor are used as reaction raw materials, acetonitrile is used as a reaction solvent, and the compound simultaneously containing the benzisothiazolinone skeleton and the benzothiazine-4-one skeleton is prepared through a one-pot method. The preparation method comprises the following steps: sequentially carrying out dimerization reaction and selective ring expansion reaction under the catalytic action of iodic acid and iodized salt, and after the reaction is finished, carrying out separation and purification to obtain a compound-N-(benzothiazinone methylene) benzoisothiazolinone which simultaneously contains a benzisothiazolinone skeleton and a benzothiazine-4-one skeleton, the method provides a new synthesis thought for preparing a derivative containing a benzisothiazolinone skeleton and a benzothiazine-4-ketone skeleton at the same time.

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 provides a preparation method and a packaging method of isoflurane, and belongs to the technical field of halogen-containing acyclic compounds. Trifluoroethanol and monochlorodifluoromethane are used as initial raw materials, a selective fluorine reagent and a NaCl solid are added, the trifluoroethanol and the monochlorodifluoromethane are etherified, under the action of the selective fluorine reagent, the obtained etherified intermediate and NaCl are chlorinated, the reaction temperature of etherification and chlorination is 60-120 DEG C, one-pot method isoflurane preparation without taking the intermediate is carried out, and the isoflurane preparation process is simplified. The preparation method is simple in steps and simple in subsequent treatment, and a high-purity product can be obtained.

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.

Provided in the present invention is a synthesis method for aprocitentan, comprising the following steps: 1) a compound of formula X and a sulfonylation reagent compound of formula XI undergoing a sulfonylation reaction to prepare a compound of formula XII; and 2) removing an R protective group on the pyrimidine sulfonamide compound of formula XII obtained in the previous step, so as to obtain aprocitentan. The synthesis method of the present invention overcomes the problem in the prior art that preparing macitentan by means of condensation of chloropyrimidine and sulfonamide needs to use an excessive amount of a strong base and involves a relatively low conversion efficiency, relatively many side products and other defects. The synthesis method does not need using a fluorine reagent for fluorination, involves economical steps, is environmentally-friendly, and has a relatively low comprehensive production cost. Compared with existing methods for preparing aprocitentan, the method of the present invention has characteristics of easily available raw materials, being environmentally-friendly and economical, and the like, thereby facilitating the industrial production of aprocitentan.

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 present invention relates to a method for catalytic hydration carbonylation of arylacetylene by using the photothermal effect of carbon nanotubes, belonging to the technical field of catalysts. This method uses a photochemical synthesis method, with a xenon lamp as the light source, carbon nanotubes (CNTs) as the photothermal material, tetrabutylammonium bromide and the selective fluorine reagent Selectfluor as additives, and under the action of Al, the hydration carbonylation of aryl alkynes is realized. When the reaction proceeds for 6 h, the separation yield of the carbonyl product is as high as 81%. This method uses photocatalysis to efficiently realize the carbonylation of alkynes under mild conditions without acid and strong oxidants.

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.