63 results about "Ethylone" patented technology

The invention discloses a preparation method and application of a photo-thermal dual-response membrane material, and relates to the field of membrane materials. When the photo-thermal double-response membrane material is prepared, a photo-thermal material firstly reacts with 4-(triethoxysilyl) aniline and then reacts with 2, 4, 6-trihydroxy-1, 3, 5-benzenetricarboxaldehyde and p-phenylenediamine, and a modified photo-thermal material is prepared; the preparation method comprises the following steps: sequentially reacting benzaldehyde with 2-hydroxyacetophenone and 3-N, N-dimethylamino methacryloyl chloride to prepare a photo-initiation monomer; the preparation method comprises the following steps: mixing N-isopropylacrylamide, a photo-initiation monomer, N, N '-methylene bisacrylamide and a modified photo-thermal material, combining with a hydrophobic substrate membrane, preparing a membrane, and finishing the surface by using 2-bromo-1-[3, 5-di (tert-butyl)-4-hydroxyphenyl] ethanone, thereby obtaining the photo-thermal dual-response membrane material. The photo-thermal dual-response membrane material prepared by the invention has the characteristics of pollution resistance, easiness in cleaning, durability, antibacterial property, metal ion recovery and low energy consumption.

The invention provides an alpha, beta unsubstituted 1, 4-ketoaldehyde compound and a metal-free photocatalytic aqueous solution acetaldehyde alpha-position selective single alkylation reaction preparation method and application thereof, a photosensitizer and alpha bromine / chloro aryl ethyl ketone are mixed in an organic solvent, then TEEDA, nBu4NI and an acetaldehyde aqueous solution are sequentially added, white light irradiation stirring reaction, separation and purification are performed, and the alpha, beta unsubstituted 1, 4-ketoaldehyde compound is obtained. Compared with the prior art, the method has the advantages that by improving the light source, the reaction can be amplified to the gram scale level, the yield of the corresponding alpha and beta unsubstituted 1, 4-ketoaldehyde product is not obviously reduced, and a basis is provided for the industrialization process of the reaction. The reaction disclosed by the invention has the characteristics of wide substrate range, high functional group tolerance, simplicity in operation, mild reaction conditions and the like. Moreover, the product disclosed by the invention can be subjected to reductive amination with cyclic secondary amine to obtain a series of gamma-aminoketones with biological activity, which shows that the reaction has potential synthesis application value in the field of pharmaceuticals.

The invention relates to the technical field of high polymer materials and protective coatings, and discloses a single-layer anti-ultraviolet heavy-duty powder coating as well as a preparation method and application thereof. The preparation method of the single-layer anti-ultraviolet heavy anti-corrosion powder coating comprises the following steps: adding carboxyl polyester resin, triglycidyl isocyanurate, modified nano silicon dioxide, modified chitosan, 2-(2H-benzotriazole-2-yl)-4, 6-di-tert-pentylphenol, bis (2, 2, 6, 6-tetramethyl-4-piperidinyl) sebacate, flaky aluminum powder, zinc phosphate, BYK-3920, 2-hydroxy-1, 2, 4-triazole-2-yl)-1, 3, 4-triazole-2-yl)-1, 3, 5-triazole-2-yl)-1, 3, 5-triazole-2-yl)-1, 3, 5-triazole-2-yl)-1, 3, 5-triazole-2-yl)-1, 3, 5- The preparation method comprises the following steps: stirring and mixing 2, 2-diphenylethanone and gamma-aminopropyltriethoxysilane at room temperature at 300-350rpm for 10-15min to obtain a mixture, extruding the mixture through a double-screw extruder at the extrusion temperature of 110-120 DEG C and the screw rotation speed of 450-500rpm, and grinding to obtain the single-layer anti-ultraviolet heavy-duty anticorrosive powder coating. The single-layer anti-ultraviolet heavy anti-corrosion powder coating can be applied to metal base material protection. The coating prepared by the invention has good ultraviolet resistance and corrosion resistance.

The invention provides a preparation method and device of prothioconazole. The preparation method comprises the following steps: carrying out Grignard reaction on o-chlorobenzyl chloride and magnesium powder in a mixed solvent of toluene and 2-methyltetrahydrofuran; the method comprises the following steps: carrying out Grignard addition reaction on a Grignard reagent and 2-chloro-1-(1-chlorocyclopropyl) ethanone; the preparation method comprises the following steps: carrying out substitution reaction on 1-chloro-2-(1-chlorocyclopropyl)-3-(2-chlorphenyl) propanol and hydrazine hydrate in an alcohol solvent; the preparation method comprises the following steps: carrying out ring closing reaction on 2-(1-chlorocyclopropyl)-1-(2-chlorphenyl)-3-hydrazino-2-alcohol, a formaldehyde solution, a sodium thiocyanate solution and a sodium hydrogen sulfate solution; the preparation method comprises the following steps: carrying out oxidation reaction on 2-(2-chlorocyclopropyl)-3-(2-chlorphenyl)-2-hydroxypropyl)-1, 2, 4-triazolidine-3-thioketone, air and inorganic alkali, so as to obtain prothioconazole. The method can improve the efficiency of the oxidation reaction and the yield and purity of prothioconazole, and is more suitable for industrial production of prothioconazole.

The invention relates to a method for simply and conveniently preparing high-purity lotinia, which comprises the following steps of: reacting 5-acetyl-3-methyl-2-thiophenecarboxylic acid with 2, 2, 2-trifluoro-1-trichlorophenyl ethyl-1-ketone to obtain 3-methyl-5-(4, 4, 4-trifluoro-3-trichlorophenyl butyl-2-enoyl) thiophene-2-formic acid, and reacting the 3-methyl-5-(4, 4, 4-trifluoro-3-trichlorophenyl butyl-2-enoyl) thiophene-2-formic acid with 2, 2, 2-trifluoro-1-trichlorophenyl ethyl-1-ketone to obtain 3-methyl-5-(4, 4, 4-trifluoro-3-trichlorophenyl butyl-2-enoyl) thiophene-2-carboxylic acid. Reacting the isoxazole thiophene formic acid compound with hydroxylamine hydrochloride to obtain an isoxazole thiophene formic acid compound; the preparation method comprises the following steps: reacting 5-[(5S)-5-trichlorophenyl-5-trifluoromethyl-4, 5-dihydro-isoxazole-3-yl]-3-methyl-thiophene-2-formic acid with (R)-1-(p-tolyl) ethyl-1-amine to obtain 5-[(5S)-5-trichlorophenyl-5-trifluoromethyl-4, 5-dihydro-isoxazole-3-yl]-3-methyl-thiophene-2-formic acid; and finally, carrying out condensation on the product and 2-amino-N-trifluoroethyl acetamide hydrochloride, so as to obtain the (5S)-configuration final product lotinib. The method has the advantages of short synthetic route, simple process, mild reaction and high chiral purity and HPLC purity, and is especially suitable for large-scale production.

The invention discloses a perillaldehyde benzyl derivative, a synthesis method thereof and application of the perillaldehyde benzyl derivative in preparation of a drug for resisting brain neuron dysfunction. According to the technical scheme, the perillaldehyde benzyl derivative is characterized in that the perillaldehyde benzyl derivative is 2-phenyl-1-(4-isopropenylcyclohex-1-ene) ethanone, the structural formula of the perillaldehyde benzyl derivative is shown in the specification, and the invention further specifically discloses a synthesis method of the perillaldehyde benzyl derivative and application of the perillaldehyde benzyl derivative to preparation of drugs for resisting brain neuron dysfunction. The perillaldehyde benzyl derivative synthesized by the invention can be used as an NMDAR2B agonist to act on NMDAR2B in a targeting manner, meanwhile, a p-PI3K / p-AKT signal channel is activated, the expression levels of NOX2 and NOX4 are inhibited, and the effect of resisting neuronal dysfunction is achieved.

The application belongs to the field of medicine synthesis, and particularly relates to a preparation method of mesopram racemate. First, 1-(4-methoxy-3-propoxyphenyl) ethan-1-one, methyl triphenylphosphonium bromide and alkali are reacted in a solvent under inert gas protection to obtain a styrene intermediate I; then the intermediate I, a BocNCl2 reagent and an alkali reagent are reacted in a solvent to generate the mesopram racemate. The method provided by the application has the advantages of short steps, low cost, no metal residue and mild reaction conditions, and is suitable for industrial production.

The present invention relates to a composition comprising 2-hydroxy-4-methoxyacetophenone (paeonol) or an isomer thereof and 4-hydroxy-3-methoxyacetophenone (acetovanillone) or an isomer thereof for use in the treatment of senescence (e.g., by modulating the mechanism of action through senescence phenotype).

The invention provides a phenolic compound with a hangover alleviating effect and a preparation method thereof. The structural formula of the polyphenol compound 1-(2, 4-dihydroxyphenyl)-2-(4-O-glucosylphenyl) ethanone is as shown in formula (I), and the polyphenol compound 1-(2, 4-dihydroxyphenyl)-2-(4-O-glucosylphenyl) ethanone is separated from pueraria thomsonii. In-vitro pharmacological experiments prove that the compound 1-(2, 4-dihydroxyphenyl)-2-(4-O-glucosyl phenyl) ethanone has good acetylcholin esterase inhibitory activity, and the EC50 value of the compound 1-(2, 4-dihydroxyphenyl)-2-(4-O-glucosyl phenyl) ethanone is 0.41 + / -0.07 mM, which indicates that the compound 1-(2, 4-dihydroxyphenyl)-2-(4-O-glucosyl The polyphenol compound 1-(2, 4-dihydroxyphenyl)-2-(4-O-glucosylphenyl) ethanone is expected to be used as a lead compound to develop a novel alcohol effect dispelling and liver protecting medicine.

The invention discloses a high-barrier puncture-resistant food packaging film and a preparation method thereof, and relates to the technical field of food packaging films. When the high-barrier puncture-resistant food packaging film is prepared, firstly, polystyrene is grafted with 2-vinylhexafluoroisopropanol, then the grafted polystyrene reacts with 2-chloro-2-oxo-1, 3, 2-dioxaphospholane, and then the grafted polystyrene reacts with 4-(dimethylamino)-2-methoxybenzonitrile to obtain modified polystyrene, and then the modified polystyrene reacts with 2-chloro-2-oxo-1, 3, 2-dioxaphospholane and 4-(dimethylamino)-2-methoxybenzonitrile to obtain the high-barrier puncture-resistant food packaging film. Secondly, reacting the pretreated vermiculite flakes with hydrogen-containing silicone oil and 1-(5-vinyl-2-hydroxyphenyl) ethanone, then reacting with phosphorus oxychloride and N, N-dimethylformamide, and then reacting with hydroxylamine hydrochloride and sodium iodide to obtain modified vermiculite flakes; and finally, carrying out melt blending on the modified polystyrene, the modified vermiculite sheets and zinc chloride, preparing into a film through a blow molding machine, and reacting with iodine and aluminum powder to prepare the high-barrier puncture-resistant food packaging film. The high-barrier puncture-resistant food packaging film prepared by the invention has good barrier property, antibacterial property and anti-aging property.

The invention discloses a continuous synthesis method of 1-(2-chlorphenyl)-2-(2-tetrazolyl) ethanone, which comprises the following steps: (1) introducing a trimethylsilylated diazomethane solution and a strong alkali solution into a micro-channel reactor 1 for reaction, introducing the obtained intermediate reaction solution and a 2-chloromethyl benzoate solution into a micro-channel reactor 2 for continuous reaction, the preparation method comprises the following steps: adding 2-chlorophenyl to generate 1-(2-chlorophenyl)-2-(2-tetrazolyl-trimethylsilane) ethanone; and (2) removing a TMS group from the 1-(2-chlorphenyl)-2-(2-tetrazolyl-trimethylsilane) ethanone, and then carrying out post-treatment to obtain the 1-(2-chlorphenyl)-2-(2-tetrazolyl) ethanone. The continuous synthesis method uses a fluid process, has the advantages of small amplification effect, high production efficiency and environmental protection, improves the selectivity of 2-tetrazole, and avoids partial sensitization of intermediates.

The application provides a preparation method of 2-aminoethyl-3-chloro-5-trifluoromethylpyridine hydrochloride, which comprises the following steps: S1: 2-acetyl-3-chloro-5-trifluoromethylpyridine is reacted with hydroxylamine and p-toluenesulfonyl chloride under alkaline conditions in a solution to obtain 1-(3-chloro-5-(trifluoromethyl)pyridin-2-yl)ethylamino p-toluenesulfonate; S2: 1-(3-chloro-5-(trifluoromethyl)pyridin-2-yl)ethylamino p-toluenesulfonate is reacted under alkaline conditions at low temperature in a solution to obtain 2-amino-1-(3-chloro-5-trifluoromethylpyridin-2-yl)ethanone; S3: 2-amino-1-(3-chloro-5-trifluoromethylpyridin-2-yl)ethanone is reduced by a reducing agent under the action of a catalyst in a solution, and finally salification is carried out to obtain 2-aminoethyl-3-chloro-5-trifluoromethylpyridine hydrochloride. The application has the beneficial effects that the total yield of three steps is 82%, the product purity is greater than 99%, the solvent can be recycled and reused, the reaction route is short, the reaction yield is high, the product purity is high, no special process is needed, and the application can be popularized in industry.

This invention discloses a purification method for 2-bromo-1-(5-iodothiophene-2-yl)-ethyl ketone. Specifically, it includes the following steps: (1) slurrying crude 2-bromo-1-(5-iodothiophene-2-yl)-ethyl ketone in solvent A; (2) slurrying the product obtained in step (1) in solvent C; and (3) recrystallizing the product obtained in step (2) in solvent D. The purification method of this invention is simple and easy to implement, yields a product with high purity, and is suitable for industrial production.

The invention discloses a preparation method of (S)-1-(3-bromopyridine-2-yl) ethanol. Specifically, the method comprises the following steps: in a liquid reaction system, taking 1-(3-bromopyridine-2-yl) ethanone as shown in a formula I as a substrate, and carrying out enzymatic reaction by using carbonyl reductase CnKRED or a mutant thereof, so as to prepare (S)-1-(3-bromopyridine-2-yl) ethanol as shown in a formula II. The preparation method disclosed by the invention has the advantages of simple process operation, low cost, high yield, high purity, easiness in large-scale production and the like. # imgabs0 #

This invention discloses an imine reductase mutant and its application in catalyzing the synthesis of amine compounds. The invention utilizes an ultra-high performance liquid chromatography (UHPLC) method to detect the source... Acidovorax Novel imine reductase Ac IRED mutation screening yielded a super mutant with high activity, high stability, and broader applicability to non-natural substrates. This mutant exhibited enhanced catalytic performance against 1-naphthyl ethylone and cyclopropylamine, and also improved activity against various ketone compounds and multiple amine nucleophiles. This invention… Ac IRED-M5 mutant activity compared to wild type Ac Compared to IRED-WT, it improved by 41.5 times, and the product... e.e. Values ​​above 99%; mutant Ac IRED-M8 mutant activity compared to wild type Ac Compared to IRED-WT, it improved by 120.5 times, with substrate conversion >90%, and product... e.e. With a value of over 99%, it has the potential for industrial applications.

This invention relates to the field of polymer materials and protective coatings, and discloses a single-layer UV-resistant heavy-duty anti-corrosion powder coating, its preparation method, and its application. The preparation method of the single-layer UV-resistant heavy-duty anti-corrosion powder coating includes: carboxyl polyester resin, triglycidyl isocyanurate, modified nano-silica, modified chitosan, 2-(2H-benzotriazol-2-yl)-4,6-di-tert-amylphenol, bis(2,2,6,6-tetramethyl-4-piperidinyl) sebacate, flake aluminum powder, and phosphorus... Zinc sulfate, BYK-392, 2-hydroxy-1,2-diphenyl ethyl ketone, and γ-aminopropyltriethoxysilane were mixed at room temperature with stirring at 300-350 rpm for 10-15 minutes to obtain a mixture. This mixture was then extruded using a twin-screw extruder at 110-120°C and a screw speed of 450-500 rpm. The mixture was then ground to obtain a single-layer UV-resistant heavy-duty anti-corrosion powder coating. This single-layer UV-resistant heavy-duty anti-corrosion powder coating can be applied to the protection of metal substrates. The coating prepared by this invention has excellent UV resistance and anti-corrosion properties.

The invention discloses a method for regulating and controlling the content of flavor components in the storage and aging process of Baijiu, and belongs to the technical field of Baijiu. The method for regulating and controlling the content of flavor components in the white spirit storage and aging process comprises the following steps: (1) uniformly mixing a catalyst and argil, adding water, mixing, molding and firing to obtain a catalytic promoter; wherein the catalyst is selected from one or more of Fe2O3 (at) SiO2-Al2O3, CuO (at) SiO2-Al2O3 and Pt-Pb (at) SiO2-Al2O3, and the catalyst is selected from one or more of Fe2O3 (at) SiO2-Al2O3; and (2) a catalytic promoter is added in the process of storing the aged white spirit in a pottery jar, and the addition amount of the catalytic promoter is 0-5% of the mass of the white spirit, but not 0. The method disclosed by the invention is beneficial to regulating and controlling the content of flavor components of the Baijiu, and particularly increasing the content of acetovanillin, vanillin, 2-methylpyrazine, 2, 3, 5, 6-tetramethylpyrazine and fenugreek lactone.

The invention belongs to the technical field of chemical synthesis, and particularly relates to a preparation method of 1-(5-methoxy-2, 3-dihydro-1, 4-benzodioxane-8-yl) ethanone. Comprising the following steps: cuprous cyanide and an initial raw material are added into N, N-dimethylformamide for nitrogen displacement, and the initial raw material is 5-bromo-8-methoxy-2, 3-dihydro-benzo [1, 4] dioxin or 5-chloro-8-methoxy-2, 3-dihydro-benzo [1, 4] dioxin; cooling after the reaction, adding ammonia water, extracting, combining organic phases, and purifying to obtain 5-cyano-8-methoxy-2, 3-dihydro-benzo [1, 4] dioxin; the preparation method comprises the following steps: reacting 5-cyano-8-methoxy-2, 3-dihydro-benzo [1, 4] dioxin with anhydrous tetrahydrofuran, dropwise adding a tetrahydrofuran solution of a methyl Grignard reagent, and reacting until no 5-cyano-8-methoxy-2, 3-dihydro-benzo [1, 4] dioxin exists; the method comprises the following steps of: extracting, concentrating and drying, and purifying to obtain the 1-(5-methoxy-2, 3-dihydro-1, 4-benzodioxane-8-yl) ethanone, namely the 1-(5-methoxy-2, 3-dihydro-1, 4-benzodioxane-8-yl) ethanone. The method has the advantages of easily available raw materials, stable process and simple operation. The method can be applied to isotope labeling synthesis of C13 and C14 compounds.

The invention provides a method for preparing resveratrol, comprising the following steps: mixing 3,5-dichlorophenylacetic acid and an acylating agent in an organic solvent and reacting the mixture to obtain 3,5-dichlorophenylacetyl chloride; then adding chlorobenzene and a catalyst to react 3,5-dichlorophenylacetyl chloride with chlorobenzene under ultraviolet light to obtain 1-(4-chlorophenyl)-2-(3,5-dichlorophenyl)ethanone; replacing chlorine in 1-(4-chlorophenyl)-2-(3,5-dichlorophenyl)ethanone to obtain 1-(4-phenol)-2-(3,5-dihydroxyphenyl)ethanone; reducing 1-(4-phenol)-2-(3,5-dihydroxyphenyl)ethanone to obtain 1-(4-phenol)-2-(3,5-dihydroxyphenyl)ethanol; and eliminating alcoholic hydroxyl groups in 1-(4-phenol)-2-(3,5-dihydroxyphenyl)ethanol to obtain resveratrol.

The invention relates to the technical field of synthesis of pharmaceutical compounds, and particularly discloses a preparation method of 1-(4-fluoro-3-pyridyl) ethanone. According to the preparation method provided by the invention, 4-aminopyridine is taken as a starting material and reacts with fluoboric acid and sodium nitrite, fluorine is firstly applied to a pyridine ring to obtain 4-fluoropyridine hydrochloride, and then the 4-fluoropyridine hydrochloride reacts with lithium diisopropylamide and N-methoxy-N-methylacetamide to obtain 1-(4-fluoro-3-pyridyl) ethanone. According to the preparation method provided by the invention, the raw materials are cheap and easy to obtain, the operation in the preparation process is simple, and the yield is high.

The invention discloses a functional polyimide yarn and a preparation method thereof, and relates to the field of fibers. When the functional polyimide yarn is prepared, amino-terminated hydrogen-containing silicone oil firstly reacts with 1-(3-allyl-2, 4-dihydroxyphenyl) ethanone, then reacts with 4, 4 '-oxydiphenylamine and 4, 4'-oxydiphthalic anhydride, is spun, and finally reacts with 4-pyridine methylsulfonyl chloride to prepare modified polyimide fibers; the preparation method comprises the following steps: carrying out surface treatment on yakwool, and then reacting the yakwool with 2-(diphenylphosphino) ethylamine, 2-bromo-1-[3, 5-di (tert-butyl)-4-hydroxyphenyl] ethanone and 4-(2-aminoethyl) pyridine in sequence to prepare modified yakwool; the modified polyimide fibers and the modified yakwool are subjected to surface treatment through a zinc acetate solution and then blended, and the functional polyimide yarn is prepared. The functional polyimide yarn prepared by the invention has good antibacterial and durable capabilities.

The present application relates to a kind of 4-(2,2,2-trifluoro-1-alkoxyethyl) phenol preparation method, it is suitable for process amplification, for industrial production, the feature of preparation method is that, including: step (1), with trifluoro-1-(4-hydroxyphenyl) ethanone as raw material, preparation intermediate A, and, step (2), intermediate A prepared in step (1) is dissolved or dispersed in alkanol B, reaction is carried out in the presence of basic substance, 4-(2,2,2-trifluoro-1-alkoxyethyl) phenol is prepared, the reaction temperature of the reaction is 50~80 DEG C, reaction time is within 3 hours.

The present invention discloses a method for preparing apremilast. The method comprises using 1-(3-ethoxy-4-methoxyphenyl)-2-(methylsulfonyl)ethanone as a raw material, subjecting the raw material to amination and reduction in the presence of a catalyst to obtain (S)-1-(3-ethoxy-4-methoxy)phenyl-2-methylsulfonylethylamine. The obtained (S)-1-(3-ethoxy-4-methoxy)phenyl-2-methylsulfonylethylamine is then reacted with 3-acetamidophthalic anhydride to obtain apremilast. The method has a short synthesis cycle, fewer reaction steps, a shortened reaction process, improved synthesis efficiency, and a high yield.

The invention provides a synthesis method of 5-methoxy-3-benzofuranone, which comprises the following steps: by taking 2-hydroxy-5-methoxyacetophenone as a raw material, firstly converting the 2-hydroxy-5-methoxyacetophenone into an intermediate 2 (2-bromo-1-(2-hydroxy-5-methoxyphenyl) ethanone), and converting the intermediate 2 into a target compound 3 (5-methoxy-3-benzofuranone) under the action of silica gel powder. According to the synthesis method, alkali is not used in key steps, and silica gel powder is used for replacing alkali, so that reaction post-treatment and purification are simple, the reaction and time cost is greatly reduced, and manufacturability amplification can be realized.

The present invention relates to processes with an improved enantiomeric excess of the desired enantiomer of the dengue viral replication inhibitor 2-(4-chloro-2-methoxyphenyl)-2- ((3-methoxy-5-(methylsulfonyl)phenyl)amino)-1-(5-(trifluoro-methoxy)-1H-indol-3-yl)ethan-1-5 one, to polymorphic forms and solvates of (S)-2-(4-chloro-2 methoxyphenyl)-2-((3-methoxy-5- (methylsulfonyl)phenyl)amino)-1-(5-(trifluoromethoxy)-1H-indol-3-yl)ethan-1-one (Compound A), to pharmaceutical compositions comprising said forms, to processes for preparing said forms, and the use of these forms.

Provided in the present invention is a preparation method for 1-[2-chloro-3-(bromomethyl)-4-(methylsulfonyl)phenyl]ethanone. A preparation method for 2-chloro-3-(trifluoroethoxymethyl)-4-(methylsulfonyl)benzoic acid of the present invention comprises: (1) in the presence of an initiator, subjecting 1-[2-chloro-3-(methyl)-4-(methylsulfonyl)phenyl]ethanone to a bromination reaction to obtain 1-[2-chloro-3-(bromomethyl)-4-(methylsulfonyl)phenyl]ethanone; (2) reacting 1-[2-chloro-3-(bromomethyl)-4-(methylsulfonyl)phenyl]ethanone to obtain 1-[2-chloro-3-(trifluoroethoxymethyl)-4-(methylsulfonyl)phenyl]ethanone; and (3) preparing 2-chloro-3-(trifluoroethoxymethyl)-4-(methylsulfonyl)benzoic acid from 1-[2-chloro-3-(trifluoroethoxymethyl)-4-(methylsulfonyl)phenyl]ethanone. The technical solution of the present invention has the advantages of involving few steps and achieving high yield, low cost and low energy consumption and the like, thus greatly reducing the production cost of tembotrione and tefuryltrione, and being more suitable for industrial production.

The invention relates to the technical field of synthesis of a 5H-dibenzo [a, d] cycloheptene skeleton, in particular to a synthesis method of the 5H-dibenzo [a, d] cycloheptene skeleton. Comprising the following steps: sequentially adding a catalyst, a ligand, alkali, a reactant I, a reactant II, a p-xylene solution and a magneton 5 into a reactor, connecting a condensing pipe, introducing condensed water from bottom to top, putting the reactor into an oil bath pan at 60-100 DEG C, heating, stirring and reacting for 6-24 hours, terminating the reaction, and purifying the product to obtain a 5H-dibenzo [a, d] cycloheptene skeleton product; the reactant I comprises 2-(2-bromophenyl)-1-acetophenone, 2-(2-bromophenyl)-1-(4-methylphenyl) ethanone, 2-(2-bromo-5-methylphenyl)-1-acetophenone or 2-(2-bromo-4-methoxyphenyl)-1-acetophenone, and the reactant II comprises 2-(2-bromophenyl)-1-(4-methylphenyl) ethanone, 2-(2-bromo-5-methylphenyl)-1-acetophenone or 2-(2-bromo-4-methoxyphenyl)-1-acetophenone; the reactant II comprises bicyclo [2.2. 1] heptyl-2, 5-diene-2, 3-dimethyl dicarboxylate, and the reactant II comprises bicyclo [2.2. 1] heptyl-2, 5-diene-2, 3-dimethyl dicarboxylate; the method is mild in reaction condition, high in selectivity, relatively high in yield and environment-friendly; the active product can be used in the field of synthesis of drugs, pesticides and paint dyes.

The invention provides a preparation method of 1-(6-methylpyridine-3-yl)-2-[4-(methylthio) phenyl] ethanone, which comprises the following steps: (1) carrying out esterification reaction on a compound 5 to obtain a compound 4, in which R is C1-C6 alkyl; (2) in the presence of an alkaline reagent, a compound 4 and a compound 3 are subjected to condensation under the catalysis of a reagent B, a compound 2 is obtained, R1 is C1-C6 alkyl, the reagent B is titanium tetrachloride, zirconium chloride, aluminum bromide or aluminum chloride, and the alkaline reagent is triethylamine, pyridine, N, N-diisopropylethylamine or N-methylmorpholine; and (3) hydrolyzing the compound 2 under an acidic condition to obtain a compound 1. According to the preparation method disclosed by the invention, high-purity 1-(6-methylpyridine-3-yl)-2-[4-(methylthio) phenyl] ethanone can be obtained at low cost, the production safety is improved, and industrial large-scale production is facilitated.

The invention discloses a preparation method of (8-bromoindolizine-3-yl) (3, 4, 5-trifluorophenyl) ketone, and belongs to the technical field of medical intermediates. The method comprises the following steps: synthesizing an intermediate 1 from 2-bromo-1-(3, 4, 5-trifluorophenyl) ethanone and 3-acetamidopyridine, generating an intermediate 2 from the intermediate 1 and maleic anhydride under the action of alkali and an oxidant, and then generating (8-bromoindolizine-3-yl) (3, 4, 5-trifluorophenyl) ketone under the action of copper bromide and t-BuONO. According to the method, 3-acetaminopyridine and 2-bromo-1-(3, 4, 5-trifluorophenyl) ethanone are adopted as raw materials, an intermediate 1 is generated, and then cyclization is performed to generate indolizine. And the cyclization is positioned between pyridine nitrogen and the amino group due to the hydrogen-bond interaction, so that the reaction design is reasonable, and an effective path is provided for the preparation of the product.