38 results about "Ethylone" patented technology

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 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 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 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.

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 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 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 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 application belongs to the technical field of organic synthetic chemistry, and particularly relates to a quinoxaline-2(1H)-selenone derivative, a preparation method and medical use thereof. The preparation method of the quinoxaline-2(1H)-selenone derivative is as follows: in an organic solvent, using o-phenylenediamine, aryl ethanone and selenium powder as raw materials, trimethylsilyl cyanide (TMSCN) as a reaction promoter, and performing a heating reaction under certain temperature conditions to obtain the quinoxaline-2(1H)-selenone derivative. The preparation method does not need to use a metal catalyst and a chemical oxidant, and has the advantages of simple operation, high yield and the like. The pharmacological activity test results show that the quinoxaline-2(1H)-selenone derivative provided by the application exhibits significant inhibitory activity on alpha-glucosidase, and has a broad application prospect in the preparation of drugs for preventing and / or treating type II diabetes, and has important significance for the development of drugs for diseases related to alpha-glucosidase mediation.

The invention discloses a ketoreductase mutant and an application of the ketoreductase mutant in preparation of (R)-1-(3, 5-dichloropyridine-4-substituted) ethanol. The ketoreductase mutant disclosed by the invention can be used for selectively reducing 1-(3, 5-dichloro-4-pyridyl) ethanone to obtain (R)-1-(3, 5-dichloropyridine-4-substituted) ethanol, the substrate concentration can reach 30 g / L, the conversion rate is greater than or equal to 98%, the ee value is greater than or equal to 98%, and the method is simple to operate and mild in reaction condition, and can be used for industrial production.

The invention relates to the technical field of preparation of compounds, in particular to a preparation method of (S)-3 ', 5'-bis (trifluoromethyl) phenyl-1-ethanol. The (S)-3 ', 5'-bis (trifluoromethyl) phenyl-1-ethanol is prepared by using a ketoreductase reduction process, the substrate of the reduction process is 3 ', 5'-bis (trifluoromethyl) phenyl-1-ethanone, and (S)-3 ', 5'-bis (trifluoromethyl) phenyl-1-ethanol is obtained by ketoreductase reduction in the presence of coenzyme. According to the preparation process, the final product is obtained through ketoreductase, the use of a dangerous and expensive CBS reduction process is avoided, and the molar yield of the final product (S)-3 ', 5'-bis (trifluoromethyl) phenyl-1-ethanol can reach 85% by optimizing reagents in the reaction process and controlling the addition amount of the reagents. The method is excellent in chiral control, mild and green in condition and suitable for industrial production.

This invention discloses a rapid distillation apparatus and processing technology for 2-chloro-1-(1-chlorocyclopropyl)ethyl ketone, relating to the field of distillation apparatus technology. The invention includes a distillation vessel body, with a steam inlet pipe fixedly connected to the lower exterior of the body. A spray device for circulating distillation of 2-chloro-1-(1-chlorocyclopropyl)ethyl ketone is installed at the top of the body, and a steam outlet pipe is fixedly connected to the top of the body. Through the cooperation of a motor, a rotating shaft, a flower-shaped baffle, a vertical Z-shaped rod, a first layered frame, a connecting plate, a second layered frame, a first slot, and a second slot, the invention ensures that 2-chloro-1-(1-chlorocyclopropyl)ethyl ketone inside the first layered frame enters the second layered frame through the first slot, and a portion of the 2-chloro-1-(1-chlorocyclopropyl)ethyl ketone flows to the bottom of the distillation vessel body through the second slot, thus forming a dispersed flow state and ensuring rapid distillation of 2-chloro-1-(1-chlorocyclopropyl)ethyl ketone.

The invention belongs to the technical field of chemical synthesis, and particularly relates to a preparation method of 1-substituted-1H-pyrazole-5-methyl formate 13C. Comprising the following steps: reacting a raw material with a substituent group, palladium acetate, 1, 1 '-bis (diphenylphosphine) ferrocene, triethylamine, methanol and N, N-dimethylformamide, replacing with nitrogen for three times, and then introducing 13CO to react; extracting and combining organic phases, washing, drying, and carrying out column chromatography purification to obtain a compound 1-substituted-1H-pyrazole-5-methyl formate 13C; the raw material with the substituent group is 1-benzyl-5-bromo-1H-pyrazole, 2-(5-bromo-1H-pyrazol-1-yl)-1-phenylacetophenone or 2-(5-bromo-1H-pyrazol-1-yl)-N, N-dimethylacetamide, and the raw material with the substituent group is one or two or more selected from a group consisting of a group consisting of 1-benzyl-5-bromo-1H-pyrazole, 2-(5-bromo-1H-pyrazol-1-yl)-1-phenylacetophenone and 2 According to the method, self-made 13CO is used as a labeling precursor, isotope labeling steps are short, reaction conditions are mild, the yield is high, and the obtained product is single and free of isomerization and generation of impurities difficult to purify.

The application discloses a kind of acetophenone derivatives and preparation method thereof, belong to organic synthesis field.The acetophenone derivative is 1-[3-methoxy-4-(1-ethyl pentyloxy) phenyl] ethanone, its preparation method includes: anhydrous tetrahydrofuran, 3-heptanol, 4-hydroxy-3-methoxy acetophenone and triphenyl phosphine are mixed, then cooling to 0~10 ℃ and keep in this temperature range drop to it azobisdimethyl valerate, after drop completion room temperature reaction 1~24 hours, again after processing is obtained.The application uses the product that can be easily purchased in market as starting material, and uses relatively safe solvent to carry out reaction, obtains higher reaction yield and high product purity, process flow operation is simple and has no harsh reaction condition, can overcome amplification effect, still maintains higher yield and high purity in kg level production, so as to be more suitable for industrialized production application.

The invention discloses a skin-friendly fabric for infants and a preparation method of the skin-friendly fabric, and relates to the field of fiber fabrics. When the skin-friendly fabric for infants is prepared, (N, N-dimethyl-3-aminopropyl) trimethoxy silane reacts with 2-(3, 4-cyclohexene oxide) ethyl trimethoxy silane and then reacts with 2-bromo-1-[3, 5-di (tert-butyl)-4-hydroxyphenyl] ethanone, and modified POSS (polyhedral oligomeric silsesquioxane) is prepared; the preparation method comprises the following steps: firstly reacting polypropylene with 5-chloro-1-pentene and styrene, and then sequentially reacting with sodium azide and 4-bromo-1-butyne to prepare functional polypropylene; zinc acetate, functional polypropylene, the modified POSS and microcrystalline cellulose are mixed, melt spinning, spinning and weaving are conducted, and the skin-friendly fabric for the infants is prepared. The prepared skin-friendly fabric for babies has flame-retardant, durable and antibacterial capabilities.

The invention discloses a method for selectively preparing an imidazo [1, 2-a] pyridine derivative by synergistically regulating rhodium catalysis through a solvent and alkali salt, which comprises the following steps: taking 2-aryl imidazo [1, 2-a] pyridine or substituted 2-aryl imidazo [1, 2-a] pyridine and alpha-chloro-aryl ethyl ketone or substituted alpha-chloro-aryl ethyl ketone as initial raw materials; the metal rhodium catalyst is used for catalyzing the carbon-hydrogen bond activation reaction to prepare the imidazo [1, 2-a] pyridine derivative, the reaction condition is mild, the selectivity and yield are high, the safety is high, and industrial production is facilitated; according to the invention, 2-aryl imidazo [1, 2-a] pyridine or substituted 2-aryl imidazo [1, 2-a] pyridine and alpha-chloro-aryl ethyl ketone or substituted alpha-chloro-aryl ethyl ketone are used as initial raw materials for the first time, a reaction is regulated and controlled by simultaneously adjusting a solvent and basic salt, and a formyl methyl imidazo [1, 2-a] pyridine compound or 6-aryl naphtho [1 ', 2': 4, 5-difluoro-2-pyridine-2-one or 6-aryl naphtho [1 ', 2': 4, 5-difluoro-2-pyridine-2-one is prepared from the same initial raw materials. According to the invention, different products of the 5, 5] imidazo [1, 2-a] pyridine compound are synthesized, and the application universality is increased.

The invention discloses a preparation method of 1-(2-chlorphenyl)-2-(2-tetrazolyl) ethanone, which comprises the following steps: (1) under the action of an ether solvent and a strong base, enabling methyl 2-chlorobenzoate to react with trimethylsilanized diazomethane to generate 1-(2-chlorphenyl)-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. According to the synthesis method, by-product isomers are reduced, the selectivity of 2-tetrazole is improved, and the total yield is further improved.

The invention discloses a preparation method of (E)-(5, 6-dihydro-[1, 4, 2]-dioxazine-3-yl)-(2-hydroxyphenyl)-ketone-O-methyl oxime, which comprises the following steps: (1) in the presence of inorganic alkali, carrying out amination reaction on 2-hydroxy-2 '-nitroacetophenone and methoxyamine hydrochloride to obtain 1-(2-hydroxyphenyl)-2-nitro-ethanone-O-methyl oxime; (2) heating the reaction system, and carrying out high-temperature cyclization, so as to obtain benzofuran-2, 3-diketone-3-(O-methyl oxime)-2-oxime; (3) supplementing inorganic alkali into the reaction system, and then adding 2-chloroethanol to carry out substitution reaction, so as to obtain benzofuran-2, 3-diketone-2-[O-(2-ethoxyl) oxime]-3-(O-methyl oxime); and (4) supplementing inorganic alkali into the reaction system, then heating to carry out high-temperature cyclization and alkaline rearrangement, and finally carrying out post-treatment to obtain the (E)-(5, 6-dihydro-[1, 4, 2]-dioxazine-3-yl)-(2-hydroxyphenyl)-ketone-O-methyl oxime. The four-step reaction yield can reach about 40%, the product purity can reach 96% or above, the quality is obviously high, and meanwhile the method is low in production cost, mild in reaction condition, simple and convenient in technological operation and suitable for large-scale industrial production.

The invention discloses a synthesis method of a psoriasis treatment drug apremilast, and belongs to the technical field of organic synthesis. The preparation method comprises the following steps: taking 1-(3-ethoxy-4-methoxyphenyl)-2-(methylsulfonyl) ethanone as an initial raw material, and carrying out reductive amination to obtain an intermediate 1; splitting the intermediate 1 by tartrate to obtain an intermediate 2; and finally, carrying out condensation reaction on the intermediate 2 and 3-acetamido phthalic anhydride to obtain apremilast. The invention develops a green and efficient synthesis process of apremilast, the preparation of a target product is realized through three-step reaction, the process breaks through the technical bottleneck that the traditional route depends on high-pressure hydrogenation conditions and noble metal catalysts (such as palladium on carbon), and the whole process adopts normal-pressure operation and mild temperature and avoids high-temperature reaction. The safety in industrial production is improved to a great extent, and the method is more suitable for industrial continuous production.