95 results about "O-aminothiophenol" patented technology

The invention discloses a fluorescent probe: a benzothiazole-terpyridine compound used for distinguishing and detecting zinc ions and cadmium ions. The probe has a structural formula as shown in (I). The compound is prepared by using bromobenzaldehyde and O-aminothiophenol as raw materials, and performing a dehydration cyclization reaction, a coupling reaction and a terpyridine derivative reaction. According to the invention, the raw materials are cheap and easily available, a synthesis route is simple, a yield is relatively high, and the fluorescent probe is high in fluorescence quantum efficiency, and relatively high in heat stability and dissolvability. The probe uses a photoinduced charge transfer mechanism, has different luminescence response for the zinc ions and the cadmium ions, has characteristics of rapid response, high sensitivity and high selectivity, is suitable for food safety inspection, laboratory safety inspection, and especially industrial wastewater monitoring, and has a wide application prospect in environment monitoring, ecological protection, disease diagnosis, industrial production and sewage inspection.

The invention discloses a benzothiazole-aniline compound used as a pH fluorescent probe and a preparation method thereof. The structural formula is shown as a chemical formula (shown in the description) (I), wherein in the formula, R1 is vinyl, acetenyl, styryl, phenylethynyl, biphenyl or perylene base; and R2 and R3 are both hydrogen, methyl or ethyl alkane. The preparation method comprises the following steps of: taking p-bromobenzaldehyde and 2-aminothiophenol as raw materials, and connecting with iodine-containing nitrobenzene derivative through dehydration cyclization reaction and coupling reaction; and generating the pH fluorescent probe benzothiazole-aniline derivative through reductive amination. Rigid structures, such as benzothiazole and phenylethynyl, are introduced into the fluorescent probe; the fluorescent probe is high in fluorescence quantum efficiency, and high in thermal stability and solubility. The probe can detect pH value under strong acid condition by adopting a photoinduced charge transfer mechanism and a conjugate passivation mechanism; and the probe has the characteristics of rapid response, high sensitivity and high selectivity, and has wide application prospect in environment monitoring, ecological protection, disease diagnosis, industrial production and sewage inspection.

The invention relates to a method for closed-loop synthesis of benzoglioxaline and benzothiazole compounds by catalytic oxidation of primary alcohol. The method comprises the following steps of: with a primary alcohol compound as an initial raw material, adding a catalyst and an oxidant and oxidizing in an organic solvent to form aldehyde; and respectively carrying out one kettle way oxidation closed-loop reaction on the aldehyde and an o-phenylenediamine compound or an o-aminobenzenethiol compound at the reaction temperature of 0-150DEG C for 1-36 hours to generate corresponding benzoglioxaline and benzothiazole compounds. The method disclosed by the invention has the advantages that the method is generally suitable for benzyl alcohol, aromatic allyl alcohol and aromatic primary alcohol containing hetero atoms such as N, O, S and the like and is simple for operation; the obtained product has high quality and higher yield; a catalyst is low in price and easily-accessible; and raw materials have low cost.

The invention relates to a fluorescent probe for detecting glutathione reductase and a bioactive sulfhydryl compound as well as a synthesis method and application thereof. In the invention, a coumarin-3-carbonyl compound with substitutional groups R1, R2, R3 and R4 is dissolved in a dry organic solvent, and o-aminothiophenol with a substitutional group R5 is slowly dropped into the mixture at room temperature or circumfluence temperature; the mixture is stirred and filtered, the organic solvent is removed, and then a probe precursor is obtained after a solid is obtained by vacuum drying; the probe precursor is dissolved in the dry organic solvent, and HgX2 is slowly dropped into the mixture under an ice bath condition; and the mixture is stirred to obtain a red solid deposit, a red solid is obtained by vacuum drying after the red solid deposit is filtered, then diffusion crystallization is carried out by using the organic solvent, and a red acicular crystal of formula (I) is obtained, i.e. the fluorescent probe. The fluorescent probe has favourable selectivity to the glutathione reductase and the bioactive sulfhydryl compound, and is suitable for the fast detection of the glutathione reductase and the bioactive sulfhydryl compound.

The invention provides a nanometer gold catalyst based on high-stability polymer, a preparation method thereof and the application thereof. The nanometer gold catalyst based on high-stability polymer, the grain size of the nanometer gold of which is 1.0nm to 5.0nm and the macromolecular protective agent of which is poly-o-amino-thiophenol, is prepared by the method as follows: o-amino-thiophenol is dissolved in a 1.0mol/L hydrochloric acid water solution, the concentration of the o-amino-thiophenol is controlled to be 0.02-0.08mol/L; after being fully stirred, the obtained solution is added with a chloroauric acid water solution at one time, and the mole ratio of the o-amino-thiophenol and the chloroauric acid is controlled to be 1:1-8:1; and then the obtained solution is fully stirred for half a minute and reacts for 12h under the temperature between 0 DEG C to 30 DEG C to obtain the stable nanometer gold catalyst of poly-o-amino-thiophenol. The nanometer gold catalyst based on high-stability polymer has the advantages that the preparation of the nanometer gold catalyst is simple and convenient to be carried out, and the obtained nanometer gold catalyst is high in stability and good in reproducibility and has good catalytic activity to the Suzuki coupling reaction between aryl halide and aryl boronic acid.

The invention relates to a novel preparation method of 2,5-dichloro-N-(2-isopropylsulfonyl) phenyl) pyrimidine-4-amine. According to the method, o-aminothiophenol is taken as the starting raw material, and 2,5-dichloro-N-(2-isopropylsulfonyl) phenyl) pyrimidine-4-amine is obtained after 5 steps including alkylation, acylation, oxidation, hydrolysis and coupling. Compared with the conventional processes, the process does not use a stinking isopropyl mercaptan reagent and is more environment-friendly. Raw materials for the whole synthesis route are easy to get, the operation of a reaction unit is simple and convenient, and the method is suitable for industrial production.

The invention provides a fluorescence probe for identifying cupric ions under an alkaline condition and a preparation method and application of the fluorescence probe, and mainly solves the problem that an existing fluorescence probe cannot quantificationally detect the cupric ions under a strongly basic condition while serving as a basic indicator. The fluorescence probe is a covalent combinationof 2-(2-hydroxyphenyl)benzothiazole and salicylhydrazide. The method comprises the steps that 1, 3-methylsalicylaldehyde and o-aminobenzenethiol react to obtain a compound 1; 2, the compound 1 obtained in step 1 reacts with urotropine to obtain a compound 2; 3, the compound 2 obtained in step 2 reacts with the salicylhydrazide to obtain a target compound Z. The fluorescence probe is used for thesensing detection of the content of the cupric ions under the strongly basic condition, and is used for the detection of pH values as a weakly basic indicator. The invention belongs to the field of fluorescence probes.

An aluminum ion and zinc ion recognition dual-functional fluorescence probe and preparation and application methods relate to dual-functional fluorescence probes and preparation and application methods thereof. The aluminum ion and zinc ion recognition dual-functional fluorescence probe and the preparation and application methods solve the problem that existing probes for independently identifyingaluminum ions or zinc ions are cumbersome in synthetic procedures and low in selectivity and sensitivity. The aluminum ion and zinc ion recognition dual-functional fluorescence probe is a covalent combination of 2-(2-hydroxyphenyl)-benzothiazole and salicylhydrazide. The preparation method of the aluminum ion and zinc ion recognition dual-functional fluorescence probe comprises, firstly, subjecting 5-methyl salicylaldehyde and o-aminobenzenethiol to reaction to obtain a compound 1; secondly, subjecting the compound 1 and urotropine to reaction to obtain a compound 2; thirdly, subjecting the compound 2 and salicylhydrazide to reaction to obtain a target compound Z. The preparation method of the aluminum ion and zinc ion recognition dual-functional fluorescence probe completes synthesis within three steps and is simple in aftertreatment process; the prepared aluminum ion and zinc ion recognition dual-functional fluorescence probe can achieve sensitive detection of aluminum ions and zincions and is good in selectivity, high in anti-interference capacity and low in detection limit. The aluminum ion and zinc ion recognition dual-functional fluorescence probe is applied to detecting heavy metal ions.

The invention discloses a preparation method of a redox probe for marking a CRP (C-Reactive Protein) impedance immunosensor. The redox probe is made of a terephthalaldehyde o-aminophenol thiophenol Schiff base nickel complex and nanogold sol. The nanogold sol in the redox probe and the sulfydryl Schiff base nickel complex have relatively strong interaction, so that stronger impedance detection signals can be provided for an unmarked CRP impedance immunosensor, and the detection performance of the immunosensor is effectively improved. The redox probe is simple to prepare and has the advantages of low detection limit, good stability, good reproducibility and the like when being used for marking the CRP impedance immunosensor to detect the CRP content.

The invention discloses a synthesis method of a 1,2,3-diazosulfide compound. A o-aminothiophenol compound with a structure shown as a formula (I) and tert-butyl nitrite are taken as raw materials, and are subjected to intramolecular diazo-reaction to obtain the 1,2,3-diazosulfide compound with a structure shown as a formula (II); a reaction equation is as follows (shown in the description), wherein R=hydrogen, fluorine, chlorine, ester group, nitro or methyl. The synthesis method has the beneficial effects that (1) the operation is simple and convenient in a preparation process, an obtained product is easy for after-treatment, and large-scale industrialized production is suitable; (2) reaction conditions are mild; (3) the synthesis cost is lowered; (4) a reaction substrate is high in functional group tolerance, is wide in range and easy to prepare; (5) the reaction is efficient, the yield is high, and the reaction efficiency is higher after reaction amplification; (6) environment pollution is avoided, and environment friendliness is achieved.

The invention discloses a bifunctional fluorescent probe for identifying copper ions and mercury ions as well as a preparation method and application thereof relates to a bifunctional fluorescent probe as well as a preparation method and application thereof, and aims at solving the problems that the existing probe for independently identifying the copper ions and the mercury ions is complex in synthesis steps, and low in selectivity and sensitivity. The bifunctional fluorescent probe is a covalent combination of 2-(2-hydroxy phenyl) benzothiazole and p-toluene sulfonyl hydrazine. The method comprises the following steps: 1, reacting 5-methylsalicylaldehyde with o-aminobenzenethiol to obtain a compound 1; 2, reacting the compound 1 obtained in the step 1 with urotropine to obtain a compound2; 3, reacting the compound 2 obtained in the step 2 with the p-toluene sulfonyl hydrazine to prepare a target compound z. The synthesis of the bifunctional fluorescent probe can be completed by onlythree steps, and the post-treatment process is relatively simple; the probe can be used for identifying both the copper ions and the mercury ions, the selectivity is good, the anti-interference capability is high, and the detection limit is low. The bifunctional fluorescent probe is used for detecting heavy metal ions.

The invention relates to the technical field of pharmaceutical chemical engineering intermediates and provides a synthesis method of a 2-arylbenzothiazole compound. The synthesis method comprises the following steps: (a) orderly adding an o-aminophenylthiophenol derivative, an aryl nitrile derivative and a protonic acid catalyst to a Schlenk bottle, putting the Schlenk bottle into oil bath for heating for reacting for 14 hours, and controlling the temperature within the range of 25-120 DEG C, wherein the molar ratio of the o-aminophenylthiophenol derivative to the aryl nitrile derivative is 1: 1, and the molar ratio of the o-aminophenylthiophenol derivative to the protonic acid catalyst is 1: (0.01-0.2); (b) after the reaction is ended, taking water and ethyl acetate as an extracting agent for extracting, and drying the organic phase after extracting by use of anhydrous Na2SO4, thereby obtaining a coarse target product benzothiazole; and (c) recrystallizing the coarse target product benzothiazole, and filtering by use of filter paper after white crystals are completely separated out, thereby obtaining the 2-arylbenzothiazole compound. The synthesis method is simple in steps, easily available in raw materials and mild in reaction conditions.

The invention belongs to the technical field of fluorescence spectrum detection and analysis, and particularly relates to a visual organic molecular fluorescence probe on the basis of cyanine and a method for preparing the visual organic molecular fluorescence probe. The visual organic molecular fluorescence probe comprises a cyanine fluorophore and benzothiazole groups. The method includes stepsof (1), dropwise adding phosphoryl chloride into N, N'-dimethylformamide to obtain mixtures, then adding the mixtures into bromoacetic acid and carrying out reaction to obtain products II; (2), carrying out reaction on 2, 3, 3'-trimethyl indole and ethyl iodide to obtain products III; (3), dropwise adding piperidine into the products II and the products III and carrying out reaction to obtain products IV; (4), carrying out reaction on the products IV and aminothiophenol at the room temperature to obtain the visual organic molecular fluorescence probe. The visual organic molecular fluorescenceprobe and the method have the advantages that obvious color change of the visual organic molecular fluorescence probe can be seen in natural light or ultraviolet lamps, linear relations between the fluorescence intensity and peroxynitrite negative ions are established, and accordingly the peroxynitrite negative ions can be qualitatively and quantitatively detected; the visual organic molecular fluorescence probe is good in selectivity and high in sensitivity, detection methods are easy to implement, and obvious effects can be realized.

The invention discloses a Schiff base based on an electron-deficient group benzothiadiazole and a preparation method of the Schiff base. A Schiff base 1 (Schiff 1) and the Schiff base (Schiff 2) containing the electron-deficient group benzothiadiazole are synthesized by using 4-bromotriphenylamine, 4-diphenylaminophenylboronic acid, 4-formylbenzeneboronic acid, 4,7-dibromo-2,1,3-benzothiadiazole and o-aminothiophenol as raw materials; and the synthesized intermediate and product are subjected to characterization by infrared spectroscopy (IR), ultraviolet-visible absorption spectroscopy (UV-vis), fluorescence spectroscopy (FS), hydrogen spectroscopy of nuclear magnetic resonance (1H NMR), carbon spectroscopy of nuclear magnetic resonance (13C NMR) and mass spectrometry (MS). The prepared Schiff base by the invention can be used for a mercury ion detecting sensor.

The invention belongs to the field of fine chemical engineering, and relates to a synthesis method of a benzothiazole compound and a related chemical technology. The method is characterized in that aminothiophenol and a 1, 3-dicarbonyl compound are used as raw materials, and the benzothiazole compound is synthesized under catalysis of protonic acid. The invention mainly aims to provide a novel method for synthesizing the benzothiazole compound. The method has the advantages that the reaction condition is mild, the method steps are simple, the raw materials are easy to obtain, the functional group compatibility is good and the like. Benzothiazole is an important biological active group and has a very wide application in the pharmacy field, so that the method has greater use values and social and economical benefits.

The invention discloses a catechol detection sensor, which relates to electron conductive polymer o-aminophenol polymer membrane modification electrode and its process method, and is applied to detection for water pollutant and neurotransmitter catechol.The sensor comprises inert electrode base and conductive polymer modification membrane, wherein, conductive polymer modification membrane is emulsion polymerisate polymer o-aminophenol and polymer adhesion amount on the surface of base electrode is 0.3í½1.5mgíñcm-2.The method comprises following steps: putting PAT(HCl) mixed with alcaine in N,N-dimethyl formamide; coating polymer liquor on electrode surface and drying it; then conducting periodic voltampere scan for polymer membrane modification electrode in 1.0mol/L acid medium.

The invention provides a fluorescent probe for detecting peroxynitrite. The probe has a general structure formula Ia or Ib. The probe is prepared by: (1) stirring R4-substituted o-aminothiophenol or R4-substituted o-aminophenol and R1/R2-substituted benzaldehyde in a methanol solution at a room temperature for two hours to obtain Ia; and (2) performing oxidative condensation of R4-substituted o-aminothiophenol or o-aminophenol and R2-substituted o-hydroxybenzaldehyde to obtain a benzothiazole or benzoxazole intermediate, coupling triflate converted by the phenolic hydroxyl group of the intermediate and R3-substituted p-hydroxybenzene tert-butyldimethylsilylester/p-aminobenzene tert-butyldimethylsilylester, and performing methylation of aniline nitrogen atoms and hydroxy elimination of silylester protecting group to obtain Ib. The fluorescent probe provided in the invention can have fast specific reaction with peroxynitrite to generate a product with strong fluorescence, so that specific detection of peroxynitrite is realized. The general structure formula of the probe in the invention is shown in the description.

This invention is a synthesis method of electron conduction polymer poly near amino thiophenols. It relates to an electron conduction polymer, especially a synthesis method of electron conduction polymer poly near amino thiophenols. It provides a synthesis method of electron conduction polymer poly near amino thiophenols. Poly near amino thiophenols is synthesized through emulsion aggregation method. Procedures are that HCl solution and dodecyl sodium sulphate are added into polymerise tank, then heated until dodecyl sodium sulphate is dissolved, poly near amino thiophenols is added, then HCl solution of ammonium persulfate is added to reaction system, then the reaction liquor is standing. Ethanol is added to the reaction liquor until emulsion breaking and polymer deposited and evolved, filtrated, scrubbed and dried. The PAT synthesized by emulsion method reduces oxidation degree of SH on PAT benzene ring, and enlarge the molecular weight of polymerisate.

The invention provides a method for selectively synthesizing a diltiazem chiral intermediate. P-methoxy cinnamyl aldehyde is used as a main raw material, firstly performs aldolization reaction with tartaric ester to produce an intermediate product 1, then epoxidation reaction is performed with hydrogen peroxide to form an intermediate product 2, oxidization is performed under acidic conditionby using potassium permanganate to obtain an intermediate product 3, ring closing reaction is performed with 2-amino-4-chloro thiophenol after purification to obtain (2S-cis)-(+)-2,3-dihydrogen-3-hydroxyl-2(4-methoxyphenyl)-1,5-benzosulfoazepine-4 (5H)-ketone, the total yield is up to 88.2%, and the optical purity is up to 99.1%.