39results about How to "Suitable for a wide range of substrates" patented technology

The invention relates to an asymmetric hydrogenation synthetic method of a chiral aromatic amine compound of iridium-catalyzed imine with high steric hindrance. The catalyst adopted is a catalyst generated by in-situ reaction of a 1, 5-cyclooctadiene iridium chloride dimer and a chiral phosphine-phosphoramidite ligand. The reaction can be carried out under the following condition: the additives comprise iodine, potassium iodide and tetrabutyl ammonium iodide; the temperature is 0-200 DEG C; the solvent is dichloromethane, 1, 2-dichloroethane to the like; the pressure is 10-100 barometric pressures; the time is 12-48 hours; and the proportion of a primer and the catalyst can reach 100000 / 1. The method provided by the invention has the characteristics of mild reaction condition, high activity, high stereoselectivity, wide application range of the primer and the like.

The invention discloses a synthetic method for preparing allyl indole compounds. A conjugated diene compound represented by formula I, a compound represented by formula II and indole compounds represented by formula III are used as reaction raw materials, an indium catalyst, Ag2CO3 and an organic solvent are added, the reaction raw materials are heated, stirred and reacted under inert gas protection conditions, and post-treatment is carried out after a result of TLC or GC-MS monitoring shows that the reaction is completed in order to obtain the allyl indole compounds represented by formula IV.The method has the advantages of easily obtained sources of the raw materials, simple process route, mild reaction conditions, low process cost, wide substrate adaptation range and high target product yield.

The invention discloses a synthetic method for a furan coupling compound. The synthetic method comprises the following steps: by taking substituted furan as a starting raw material, palladium trifluoroacetate or palladium acetate as a catalyst and oxygen as an oxidant, carrying out one-step synthesis in an organic solvent to obtain a substituted furan coupling product. According to the method, furan coupling directly oxidized by a C-H bond can be realized, the method is simple to operate compared with the traditional method, a substrate application range is wider, the reaction efficiency is higher, and the method is environmentally-friendly, high in yield and high in atom utilization rate.

The invention discloses a preparation method of an E-vinyl sulfones compound. The preparation method comprises the following steps: dissolving raw materials of olefin and thiophenol (thioalcohol) into a tetrahydrofuran solvent; then adding lodine pentaoxide and organic base DBU (1,8-diazabicyclo undec-7-ene); directly reacting for 12 to 16 hours under 60 to 80 DEG C; separating and purifying a coarse product after stopping reacting, thus obtaining the E-vinyl sulfones compound. The preparation method has the advantages that raw materials are simple and can be easily obtained, the price is cheap, the reaction requires no metal catalyst, metal pollution is avoided, the operation is simple and is free of harsh conditions of water free, oxygen free and the like, the adaptive range of a substrate is wide, the reaction stereoselectivity is high, the process conditions are stable, and a prepared product is easy to purify.

The invention discloses a reparation method of a sulfonamides compound. The preparation method includes: using thiophenol and amine which are simple and easy to get as raw materials; enabling the raw materials to be in direct oxidation coupling reaction under mediation of safe and stable iodine pentoxide to prepare sulfonamide. The preparation method has the advantages that reaction conditions are mild (60 DEG C), the raw materials are simple and easy to get and low in price, reaction environment is friendly, a substrate is wide in application range, and metal catalysts and harsh reaction conditions like low or high temperature and zero water and zero oxygen are not needed, so that metal pollution related to common synthesis methods is avoided; the preparation method further has the advantages of simple, convenient and safe operation, stable process condition and easiness in product purification and is suitable for large-scale production.

The invention discloses a synthetic method for a cannabinol compound. The synthetic method comprises the following steps: subjecting two aryl carbon-hydrogen bonds to direct coupling by one step so as to synthesize a 6H-benzo[c]chromene compound with 3,5-dihydroxypentylbenzene as a starting material, palladium acetate as a catalyst and oxygen as an oxidant under the protections of phenolic hydroxyl benzyl and 2-pyridylsulfonyl, and carrying out oxidation, deprotection and methylation so as to synthesize cannabinol with high yield. The method provided by the invention realizes that direct oxidation and aryl coupling through C-H bond activation are used as the key steps of synthesizing the cannabinol, so highly-efficient and simple synthesis of the cannabinol is realized. Compared with a traditional method, the method provided by the invention has the advantages of simple operation, higher reaction yield, environment friendliness and high atom utilization rate.

The invention discloses a method for determining residue of methaqualone and diazepam in animal-derived food like pork, fish, pig liver and pig kidney. The method includes: adopting ethyl acetate as an extraction solvent; purifying through a mixed powder pipe; using a liquid chromatography-tandem mass spectrometer for detection; adopting an internal standard method for quantification. Regression equation correlation coefficient reaches higher than 0.99, determination lower limit is 0.5ug / kg, recycling rate on adding concentration level of 0.5-5ug / kg is 90-120%, and relative standard deviation in a lab is lower than or equal to 15%. The method is simple and convenient to operate, high in sensitivity and interference resistance, wide in matrix adapting range, scientific and accurate in qualification and quantification, suitable for quick analysis of mass samples and capable of meeting technical requirements of related supervision departments of China.

The invention discloses an effective regioselectivity and diastereoselectivity method. A trans-3, 4-diaryl dihydrocoumarin compound is prepared through [4 + 2] cyclization reaction of alkyne amine and o-hydroxybenzyl alcohol under the condition of non-metal catalysis. Alkyne amine is used as a 2-pi partner and reacts with o-hydroxybenzyl alcohol through the positioning effect of sulfonamide, and various trans-3, 4-diaryl dihydrocoumarin compounds are prepared with good yield and high regioselectivity and diastereoselectivity. The non-metal catalytic reaction method has a wide substrate application range and good functional group tolerance, and can be used for efficiently producing in a gram scale.

The invention discloses a trans-olefin compound synthesis method, which comprises: carrying out a heating reaction on an alkyne compound represented by a general formula (I), a reducing agent and a solvent to obtain a trans-olefin compound represented by a general formula (II), wherein the synthesis route is as follows: R1 and R2 are independently selected from hydrogen, alkyl, cycloalkyl or aryl;wherein the reducing agent is a sulfur-containing compound and is selected from at least one of thioacetamide, N,N-dimethyl dithiocarbamate dimethyl ammonium salt, dimethyl amino sodium dithioformatedihydrate, potassium ethyl xanthate and potassium isopropyl xanthate. According to the method, a cheap, efficient and safe reducing agent is utilized to realize high-selectivity reduction of alkyne to prepare trans-olefin under the condition of no transition metal catalysis, so that the method is simple and easy to implement, wide in substrate application range and easy to realize industrialization.

The invention a determination method of benzimidazoles drug residue in chicken, chicken liver and chicken kidney. The determination method comprises the step of simultaneously determining residues ofnine benzimidazoles drug residual markers in the chicken, chicken liver and chicken kidney by adopting high-performance liquid chromatography, and the technical blank at this field is filled. A regression equation related coefficient of the method reaches 0.999 and more, the lower determination limit is 50 micrograms / kg, the recovery rates on different adding concentration levels are 75%-110%, andthe relative standard deviation in the experiment is not more than 15%. The technical problem of simultaneously determining nine benzimidazoles drugs is solved, the determination has the originalityon the pre-treatment technology of the sample, especially on the purification technology. The method is scientific and accurate in quantification, strong in interference resistance, wide in matrix adaption range, and capable of satisfying the latest technical requirement of the related supervision department of our country.

The invention discloses a preparation method of a chiral epoxy compound. The preparation method is characterized by preparing the chiral epoxy compound by catalyzing alpha, beta-unsaturated ketone to be subjected to asymmetric epoxidation reaction by adopting a chiral bridging aryloxy alkoxy rare-earth compound as a catalyst; the general formula of the catalyst is [LnL2][{(THF)3Li}2(mu-Cl)], the chemical structural formula of the catalyst is as shown in the specification, wherein Ln is one of rare-earth metals, namely neodymium, samarium, ytterbium, yttrium and lutetium, and L=(S)-2,4-di-tert-butyl-6-((2-(hydroxydiphenylmethyl)pyrrolidin-1-yl)methyl)-phenol. The method disclosed by the invention has the advantages of easiness for catalyst synthesis, convenience for separation and purification, low raw material cost and mildness in reaction condition; the chiral epoxy compound prepared through the method has the advantages of high catalytic activity, good enantioselectivity and wide substrate application range.

The invention discloses a method for preparing an alpha-acyloxy ketone compound. According to the invention, simple and easily available alcohol and carboxylic acid are taken as the raw materials, under mediation of NBS(N-bromo-succinimide) and DBU(1,8-diazabicyclo(5.4.0)undec-7-alkene), the alpha-acyloxy ketone is prepared by a one-pot reaction. The method has the advantages of mild reaction condition, simple and easily available raw materials, wide substrate adaptation scope, no requirement of rigorous reaction conditions such as any metal catalyst, peroxy compounds, low or high temperature and water-free and oxygen-free conditions, metal pollution is avoided; and the method also has the advantages of stable technical condition, simple and safe operation, and easy purifying of the product.

The invention discloses a synthesis method of chiral gamma-amine methylene-gamma-butylene lactone compound, and belongs to the technical field of organic synthesis. According to the synthesis method,Schiff base, a chiral organic small molecular catalyst, and an auxiliary agent are dissolved in anhydrous toluene, an obtained mixture is stirred for 10 to 20min; under nitrogen protection, 2-(trimethyl siloxy)furan is added into an obtained reaction system, an obtained reaction mixture is subjected to column chromatography purification so as to obtain the chiral gamma-amine methylene-gamma-butylene lactone compound. In the synthesis method, Schiff base and 2-(trimethyl siloxy)furan are subjected to asymmetric vinylogy Mannich, product yield is 90% or higher, the highest enantioselectivity is97%, the highest diastereoselectivity is 93:7, and the synthesis method is capable of realizing high efficiency of synthesis of chiral gamma-butylene lactone containing gamma site amine methylene.

The invention discloses a novel method for synthesizing a 2H-azirines derivative. The method comprises the following steps: adding an alkyne compound shown as a formula I and sodium sulfonate shown asa formula II into a Schlenk sealing pipe reactor in sequence; then adding tert-butyl nitrite (t-BuONO) and an organic solvent; heating and stirring to react in an oil bath under a protection condition of an inert atmosphere; after finishing TLC or GC-MS monitoring reaction, carrying out post-treatment to obtain the 2H-azirines derivative shown as a formula III. The method has the advantages of easiness of obtaining raw material sources, simple technological route, moderate reaction conditions, low technological cost, wide substrate applicable range and high yield.

The invention discloses a chiral bridged aryloxyalkyloxy scandium chloride. The chiral bridged aryloxyalkyloxy scandium chloride is characterized in that the chiral bridged aryloxyalkyloxy scandium chloride has a general formula of LScCl(THF), and has a chemical structural formula shown in the specification, and L is (S)-2,4-di-tert-butyl-6-((2-(hydroxydiphenylmethyl)pyrrolidin-1-yl)methyl)-phenolate. The above compound has the advantages of simple synthesis, clear structure and high yield. The invention also provides a preparation method of the compound, and an application method of the compound in the catalysis of the asymmetric hydrogen phosphorization reaction of alpha, beta-unsaturated ketone as a catalyst. The application method has the advantages of mild conditions, high selectivity, good antipodal selectivity and wide substrate adaptation range.

The invention discloses a synthesis method of an ester compound. The method comprises the following steps: carrying out an oxa-Michael addition reaction by using organic carboxylic acid and alpha,beta-unsaturated ketone as initial raw materials and a sodium carbonate aqueous solution as a reaction medium to synthesize the ester compound. Compared with the traditional ester compound synthesis method, the method provided by the invention has the advantages of mild reaction conditions, simple operation, low reagent price, wide substrate application range, environmental friendliness, high yield and complete atom utilization.

The invention provides a benzothiophene compound as well as a preparation method and an application method thereof, and belongs to the technical field of heterocyclic compound synthesis. The preparation method comprises the following steps: taking acetone as a solvent, DTPB as a free radical initiator and a 2-ethynylphenylthioether derivative as a raw material, carrying out a one-step reaction ina nitrogen atmosphere in the presence of sodium dihydrogen phosphate to prepare a crude product, and refining the crude product to obtain the benzothiophene compound. The prepared compound is a new compound, the steps are short, the operation is simple, the cost is low, and a universal new method is provided for the preparation of benzothiophene compounds.

The invention discloses a synthetic method of 2-thiophenylbenzoic acid. The synthetic method is characterized by including the steps of: 1) dissolving raw materials, comprising phenylboric acid represented as the formula I and thiosalicylic acid represented as the formula II, in an alkaline solution and adding anhydrous ethylenediamine; 2) in the presence of a metal salt catalyst and a ligand, carrying out a heating reaction at higher than 100 DEG C for more than 16 h with TLC tracing detection, and when then reactant, thiosalicylic acid, disappears, the reaction is determined to be finished; 3) naturally cooling the mixture to room temperature to obtain a mother liquid, extracting the mother liquid with ethyl acetate, drying an organic layer with anhydrous magnesium sulfate, and performing reduced-pressure rotary evaporation to remove the solvent and obtain a solid; and 4) purifying the solid crude product through a silica gel column, collecting an eluent, and performing rotary evaporation to dry the eluent to obtain the 2-thiophenylbenzoic acid represented as the formula III. The method is simple in reaction conditions and high in yield, is easy to enlarge in large scale, and is environment-friendly and low-pollution.

The invention relates to the field of drug residue detection, in particular to a purification filler for sulfonamide drug residues, a solid-phase purification column containing the filler and a corresponding pretreatment method. According to the solid-phase purification column and the pretreatment method, the adsorption principle of the mixed filler is utilized, various impurities in the to-be-detected sample can be simply and quickly removed, the operation is simple and convenient, and a detection result with good stability and high recovery rate is ensured to be obtained under the condition that calibration of a matrix standard curve is not needed.

The invention discloses a reparation method of a sulfonamides compound. The preparation method includes: using thiophenol and amine which are simple and easy to get as raw materials; enabling the raw materials to be in direct oxidation coupling reaction under mediation of safe and stable iodine pentoxide to prepare sulfonamide. The preparation method has the advantages that reaction conditions are mild (60 DEG C), the raw materials are simple and easy to get and low in price, reaction environment is friendly, a substrate is wide in application range, and metal catalysts and harsh reaction conditions like low or high temperature and zero water and zero oxygen are not needed, so that metal pollution related to common synthesis methods is avoided; the preparation method further has the advantages of simple, convenient and safe operation, stable process condition and easiness in product purification and is suitable for large-scale production.

The invention provides a preparation method for an indole compound, and belongs to the technical field of preparation of heterocyclic compounds. The preparation method comprises the following steps: with 1,2-dichloromethane as a solvent, silver oxide as a catalyst and 2-ethynylaniline and derivatives thereof as raw materials, subjecting the raw materials to a complete reaction at 10 to 60 DEG C inthe presence of p-toluenesulfonic acid monohydrate, carrying out spin-drying so as to obtain a crude product, and carrying out column chromatographic separation so as to obtain a fine product namelythe indole compound. The preparation method provided by the invention has the advantages of short preparation steps, mild reaction conditions, high product yield and low cost, and provides a universalnovel method for preparation of the indole compound.

The invention discloses a method for determining the residual amount of benzimidazoles in chicken, chicken liver and chicken kidney. The present invention provides for the first time the simultaneous determination of the residues of nine benzimidazole drug residue markers in chicken, chicken liver and chicken kidney by using high performance liquid chromatography, which fills the technical gap in the art. The correlation coefficient of the regression equation of the present invention reaches more than 0.999, the lower limit of determination is 50 μg / kg, the recovery rate at different concentration levels is 75% to 110%, and the relative standard deviation in the laboratory is ≤15%. The present invention solves the technical problem of simultaneous determination of nine kinds of benzimidazole drugs, and has originality in the sample pretreatment technology, especially in the purification technology. Meet the latest technical requirements of relevant regulatory authorities in my country.

The invention discloses a synthesis method of cannabinoid compounds. The steps are as follows: 3,5-dihydroxypentylbenzene is used as a starting material, protected by a phenolic hydroxybenzyl group, protected by a 2-pyridylsulfonyl group, and palladium acetate is used as a catalyst. Oxygen is used as the oxidizing agent, and two aryl carbon-hydrogen bonds are directly coupled to synthesize 6H-benzo[c]chromene compounds in one step, and then through oxidation, deprotection, and methylation, cannabidiol can be synthesized with high yield. The method of the present invention realizes direct oxidative aryl coupling through C-H bond activation as a key step in the synthesis of cannabinol, and can synthesize cannabinol efficiently and concisely. Compared with traditional methods, it is simple to operate, has higher reaction yield, is environmentally friendly, and has high atom utilization rate.

The invention relates to the field of organic synthesis, and concretely relates to a preparation method of a 5-sulfonyl oxy-8-carboxamidoquinoline derivative, in particular to the method for preparing the 5-sulfonyl oxy-8-carboxamidoquinoline derivative by adopting 8-acetamido quinoline as a raw material. The method is characterized by comprising the steps of adopting trifluoroacetic acid iodobenzene as an oxidizing agent, carrying out C-H functionalization reaction on 8-carboxamidoquinoline and various different N,N'-disulphohydrazide compounds under metal-free catalysis, and obtaining a C5-site sulfonyl oxy substituted product. Compared with the document, the preparation method provided by the invention has the characteristics that the raw materials are easily obtained, the substrate adaption range is wide, the yield is high and the like.

The invention discloses a synthetic method of 2-thiophenylbenzoic acid. The synthetic method is characterized by including the steps of: 1) dissolving raw materials, comprising phenylboric acid represented as the formula I and thiosalicylic acid represented as the formula II, in an alkaline solution and adding anhydrous ethylenediamine; 2) in the presence of a metal salt catalyst and a ligand, carrying out a heating reaction at higher than 100 DEG C for more than 16 h with TLC tracing detection, and when then reactant, thiosalicylic acid, disappears, the reaction is determined to be finished; 3) naturally cooling the mixture to room temperature to obtain a mother liquid, extracting the mother liquid with ethyl acetate, drying an organic layer with anhydrous magnesium sulfate, and performing reduced-pressure rotary evaporation to remove the solvent and obtain a solid; and 4) purifying the solid crude product through a silica gel column, collecting an eluent, and performing rotary evaporation to dry the eluent to obtain the 2-thiophenylbenzoic acid represented as the formula III. The method is simple in reaction conditions and high in yield, is easy to enlarge in large scale, and is environment-friendly and low-pollution.

The invention relates to the field of organic synthesis, and concretely relates to a preparation method of a 5-sulfonyl oxy-8-carboxamidoquinoline derivative, in particular to the method for preparing the 5-sulfonyl oxy-8-carboxamidoquinoline derivative by adopting 8-acetamido quinoline as a raw material. The method is characterized by comprising the steps of adopting trifluoroacetic acid iodobenzene as an oxidizing agent, carrying out C-H functionalization reaction on 8-carboxamidoquinoline and various different N,N'-disulphohydrazide compounds under metal-free catalysis, and obtaining a C5-site sulfonyl oxy substituted product. Compared with the document, the preparation method provided by the invention has the characteristics that the raw materials are easily obtained, the substrate adaption range is wide, the yield is high and the like.

The invention discloses a new method for synthesizing 2H-aziridine derivatives. In the Schlenk sealed tube reactor, add the alkyne compound shown in formula I successively, the sulfonic acid sodium salt shown in formula II, add tert-butyl nitrite (t-BuONO) and organic solvent again, under inert atmosphere protection condition Next, the oil bath was heated and stirred to react, and after the completion of the reaction was monitored by TLC or GC-MS, the 2H-aziridine derivative shown in formula III was obtained through post-processing. The method has the advantages of easy source of raw materials, simple process route, mild reaction conditions, low process cost, wide substrate adaptability and high yield.

The invention discloses a preparation method of a chiral epoxy compound. The preparation method is characterized by preparing the chiral epoxy compound by catalyzing alpha, beta-unsaturated ketone to be subjected to asymmetric epoxidation reaction by adopting a chiral bridging aryloxy alkoxy rare-earth compound as a catalyst; the general formula of the catalyst is [LnL2][{(THF)3Li}2(mu-Cl)], the chemical structural formula of the catalyst is as shown in the specification, wherein Ln is one of rare-earth metals, namely neodymium, samarium, ytterbium, yttrium and lutetium, and L=(S)-2,4-di-tert-butyl-6-((2-(hydroxydiphenylmethyl)pyrrolidin-1-yl)methyl)-phenol. The method disclosed by the invention has the advantages of easiness for catalyst synthesis, convenience for separation and purification, low raw material cost and mildness in reaction condition; the chiral epoxy compound prepared through the method has the advantages of high catalytic activity, good enantioselectivity and wide substrate application range.