30 results about "Alpha-bromoacetophenone" patented technology

The invention discloses a paeonol thiazole derivative and a preparation method and application thereof. The paeonol thiazole derivative has a structure shown in a formula (I), wherein R is a benzene ring substituent, and in particular one of hydrogen atom, halogen atom, hydroxyl group, methoxy group and nitro group. The preparation method comprises the following steps of: A, performing condensation reaction on paeonol and thiosemicarbazide to synthesize paeonol thiosemicarbazide; and B, reacting the prepared paeonol thiosemicarbazide with alpha-bromoacetophenone of different substituents to obtain the paeonol thiazole derivative. By the adoption of the paeonol thiazole derivative and the preparation method and application thereof, a new paeonol thiazole derivative is provided, which has the advantages of short preparation period, simple operation, low cost, high purity and stable quality of the obtained derivative; and experiments also show that antitumor activity of the derivative canbe improved by introducing an antitumor pharmacodynamic group thiazole on a paeonol skeleton, and the derivative can be used as the antitumor derivative.

The invention belongs to the field of organic chemical synthesis technology and relates to an efficient and simple method for synthesis of a 2-amino-4-aryl-5-methylthiothiazole compound. The method of the invention comprises the following synthesis steps: (1) dissolving aryl ethylketone in a DMSO / HBr mixed system, heating and reacting to prepare alpha-bromoacetophenone dimethylsulfonium salt; and (2) dissolving the sulfonium salt prepared in the step (1) into water, adding thiourea, and stirring at room temperature; and adding ethanol, continuously heating and reacting to prepare 2-amino-4-aryl-5-methylthiothiazole.

The invention discloses a preparation method of 4-phenylimidazole. The method comprises the following steps: 1) substitution, namely, dissolving alpha-bromoacetophenone into formamidine acetate, and reacting in ethylene glycol, so as to obtain a nucleophilic replace intermediate; 2) cyclizing, namely, adding potassium carbonate as an acid-binding agent, and controlling the temperature to carry out a cyclization reaction; and 3) post-treatment, namely obtaining the 4-phenylimidazole by post-treatment after the reaction is ended. According to the technical scheme disclosed by the invention, the 4-phenylimidazole is synthetized from conventional chemical raw materials; the preparation method is simple in process, less in reaction steps, and convenient to purify; an industrial operation is facilitated; the target product is white in color and luster; the content of the final product can be up to over 99%; the yield is greater than 45%.

The invention relates to a benzofuran [2, 3-c] pyridine compound and a synthetic method thereof. The benzofuran [2, 3-c] pyridine compound has a general formula shown in the specification, wherein R1 is phenyl, 3-bromo-phenyl, 4-bromo-phenyl, 4-chloro-phenyl, 4-methoxy-phenyl, 3-methyl-phenyl or 4-methyl-phenyl; R2 is hydrogen or 5-chlorine, 5-bromine, 5-tert-butyl, 3,5-ditert-butyl, 4-methoxy, 5-methoxy, 5-methyl, 3,5-dimethyl and 4,5-dimethyl; R3 is methyl or phenyl, 4-bromo-phenyl, 3-bromo-phenyl, 2-chloro-phenyl, 4-chloro-phenyl, 4-methoxy-phenyl and 4-methyl-phenyl. According to the synthetic method disclosed by the invention, alpha-bromoacetophenone or a derivative thereof as well as 4-(2-hydroxyphenyl)-3-butylene-2-ketone or a derivative thereof are used as reactants, and a one-pot method is adopted to synthesize the benzofuran [2, 3-c] pyridine compound. The synthetic method is simple and convenient in step, mild in condition and high in yield.

The invention relates to a UV-initiated delay-curable one-component epoxy adhesive. The adhesive is prepared from the following raw materials in percentages by weight: 30-60% of epoxy resin, 5-30% of a homemade quaternary photobase generator, 10-30% of a toughening agent and 5-20% of a filling agent, wherein the homemade quaternary photobase generator is synthesized from the following components of alpha-bromoacetophenone, terephthalic acid (TPA) and sodium tetraphenylborate by the following processes: reacting alpha-bromoacetophenone and an acetone liquid of terephthalic acid (TPA) at room temperature to prepare bromo-quaternary ammonium salt, filtering, drying and recrystallizing the product to obtain a crystal substance, dissolving the crystal substance in distilled water and carrying out anion exchange reaction on the distilled water with the crystal substance and sodium tetraphenylborate at room temperature to obtain a product, washing the product with distilled water and drying to obtain anion quaternary ammonium salt paired with tetraphenylborate. Compared with the prior art, the curing speed can be delayed to 30 minutes-60 minutes, the process is simple, neither heat curing nor mixing is needed, the adhesive is environmentally friendly and is convenient to use and is also simultaneously suitable for multiple opaque materials and can be widely used in the field of structural bonding.

The invention relates to a method for measuring derivatization in a valproic acid body fluid concentration process through a high performance liquid chromatography. According to the method, triethylamine is replaced by quaternary ammonium hydroxide acetonitrile solution (tetramethylammonium hydroxide acetonitrile solution or tetrabutyl ammonium hydroxide acetonitrile solution or tetraethyl ammonium hydroxide acetonitrile solution) to catalyze valproic acid and is derived into phenyl ester which is ultraviolet detectable with a derivating agent (2,4'-dibromo acetophenone acetonitrile solution, alpha-bromoacetophenone acetonitrile solution, 2-bromo-p-nitroacetophenone acetonitrile solution or 4-bromo-7-herniarin acetonitrile solution), the derivating agent which is only 3-5 molar times that of amount of the reactants is required, and the derivatization yield above 95 percent can be achieved. The method has the advantages that the derivatization reaction is complete, the chromatogram base line is stable, endogenous impurity interference is avoided, the measurement result is accurate, the precision is high, the sensitivity is high, the using amount of the derivating agent is small, the pressure of the chromatographic column is hardly increased, and the service life of the chromatographic column is prolonged.

The invention discloses a cyclic carbonate and a preparation method thereof. The formula of the cyclic carbonate related by the invention is disclosed in the specification. The preparation method comprises the following steps: dissolving benzaldehyde or derivatives thereof and alpha-bromoacetophenone or derivatives thereof in an anhydrous dioxane solution; introducing carbon dioxide gas at the flow rate of 200-300 ml / min under atmospheric pressure at 10-55 DEG C while stirring; dropwisely adding diisopropyl lithium amide into the solution; leading the reaction system completely to react underthe conditions of stable carbon dioxide gas flow; and after the reaction finishes, quenching the reaction with saturated ammonium chloride solution, extracting with ethyl acetate, drying to remove the solvent, and carrying out silicagel column chromatography to obtain the target product.

The invention discloses a method for synthesizing alpha-bromo acetophenone compound, which comprises the steps: hydrosulphite solution is added into the mixture of substituted phenylethanone and bromate at the temperature of 30-90 DEG C, and the mixture is stirred to react for 2-9h, and then is cooled, filtered, washed and dried, so that the alpha-bromo acetophenone compound is obtained. The method also has the advantages that the product has high product purity, the price of bromide reagent is low, aqueous phase is solvent instead of organic solvent, the pollution is little, the operation issimple, and the method is suitable for mass production.

The invention discloses a novel synthesis method for 3-nitryl-4-benzyloxy-alpha-bromoacetophenone having a structure represented by the formula (I), comprising the steps of: taking 3-nitryl-4-benzyloxyacetophenone having a structure represented by the formula (II) as raw material and taking phosphor or halide thereof as a catalyst; dissolving at first the 3-nitryl-4-benzyloxyacetophenone having the structure represented by the formula (II) and the catalyst in a reactive solvent; dropwise adding a mixed solution of bromine and the reactive solvent while maintaining the temperature in a range from negative 5 to 10 DEG C, after the addition, reacting for 1-5 hours while maintaining the temperature in a range from negative 5 to 10 DEG C, and filtering, washing and drying to obtain the 3-nitryl-4-benzyloxy-alpha-bromoacetophenone; the reactive solvent is selected from one of the group consisting of: ethyl acetate, methanol, ethanol, methylene dichloride, methenyl chloride, ethylidene dichloride and methylbenzene. The invention is mild in reaction conditions, friendly in reaction environment, short in reaction time, high in product yield and suitable for industrial production.

The invention discloses a synthesis method of an alpha-acyl homoallyl thioether compound. A series of alpha-acyl homoallyl thioether compounds with application value are finally synthesized by adopting a three-component and one-pot method, taking an alpha-bromoacetophenone compound, a thiol compound and an allyl bromide compound as reactants, taking inorganic salt as an additive, taking an ultra-dry or anhydrous inorganic solvent as a solvent and reacting at the temperature of 60 DEG C to 130 DEG C. The synthesis method disclosed by the invention has the beneficial effects that a series of the homoallyl thioether compounds with the potential application value are synthesized in high yield, and the utilization of a transition metal catalyst and a diazo compound can also be avoided; meanwhile, additives including strong acid, strong alkali and the like are not needed in a reaction process, and the protection of inert gas is not needed; the after treatment of reaction is simple.

The invention discloses a high-selectivity synthesis method of benzoyl formic acid, which comprises the following steps: oxidizing styrene, which serves as the raw material, in a H2O2 / tetrabutylammonium bromide mixed system to generate alpha-bromophenethyl alcohol; oxidizing the generated alpha-bromophenethyl alcohol with H2O2 to generate alpha-bromoacetophenone; hydrolyzing the alpha-bromoacetophenone under alkaline conditions to generate alpha-hydroxyacetophenone; and oxidizing the alpha-hydroxyacetophenone with H2O2 to generate the target product benzoyl formic acid. In the invention, oxydol is used as an oxidant, and the byproduct is water, thereby reducing the generation of the organic byproducts and the discharge amount of inorganic salt (acid) waste water. Compared with other inorganic heavy metallic salt and inorganic mineral acid oxidization methods, the method disclosed by the invention enhances the cleanness of industrial preparation reaction, and reduces the environmental pollution. The invention enhances the product yield and purity: the yield is enhanced by nearly 13%, the total yield is up to 93.7%, and the product purity exceeds 95%; and other indexes are correspondingly enhanced.

The invention discloses a high selectivity synthesis method of benzoyl formic acid. With styrene as raw material, addition oxidation reaction is carried out in a mixed system of H2O2 and tetrabutyl ammonium bromide to obtain alpha-bromoacetophenone; then ethylene glycol and para-toluenesulfonic acid are added, reflow reaction is carried out to generate alpha-bromoacetophenone ethylene glycol; thegenerated alpha-bromoacetophenone ethylene glycol is hydrolyzed in potassium carbonate solution to generate alpha-hydroxyacetophenone ethylene glycol; the alpha-bromoacetophenone ethylene glycol reacts in the mixed system of H2O2 an tetrabutyl ammonium bromide to obtain 2-phenyl-1,3-dioxolame-2-carboxylic acid, and then deprotection reaction is carried out with oxalic acid to generate target product benzoyl formic acid. The synthesis method disclosed by the invention has high reaction yield, good reaction selectivity, low cost, simple technological process, mild reaction conditions and high product purity, and the defects of the traditional technological method that environment is severely polluted and cost is high are overcome, thus the synthesis method disclosed by the invention has industrial-scale production prospect.

The preparation method for alpha-hypnone bromide comprises: stirring and heating to 90Deg, dripping the liquid bromine directly into hypnone compound aqueous solution to produce the product as an important drug intermediate and HBr gas. This invention is practical, belongs to a green chemical method without any toxic organic solvent, and has great economic value.