33 results about "P-Anisidine" patented technology

The present invention provides, according to an aspect thereof, a novel process for the preparation of dronedarone [1] and pharmaceutically acceptable salts thereof. According to a preferred embodiment, the process comprises N-acetylating of p-anisidine or p-phenetidine with acetic anhydride, reacting of the obtained N-(4-alkoxyphenyl)acetamide with 2-bromohexanoyl chloride or bromide in the presence of aluminum chloride or bromide to obtain N-[3-(2-bromohexanoyl)-4-hydroxyphenyl]acetamide [6a], converting the compound [6a] into 2-butyl-5-benzofuranamine hydrochloride [12a] and subsequently converting [12a] into [1] or pharmaceutically acceptable salts thereof. In accordance with another aspect of this invention, there are provided novel intermediates, inter alia the novel compounds [6a] and [12a]. The novel intermediates of the present invention are stable, solid compounds, obtainable in high yields, which can be easily purified by crystallization and stored for long periods of time.

The present invention provides, according to an aspect thereof, a novel process for the preparation of dronedarone [1] and pharmaceutically acceptable salts thereof. According to a preferred embodiment, the process comprises N-acetylating of p-anisidine or p-phenetidine with acetic anhydride, reacting of the obtained N-(4-alkoxyphenyl)acetamide with 2-bromohexanoyl chloride or bromide in the presence of aluminum chloride or bromide to obtain N-[3-(2-bromohexanoyl)-4-hydroxyphenyl]acetamide [6a], converting the compound [6a] into 2-butyl-5-benzofuranamine hydrochloride [12a] and subsequently converting [12a] into [1] or pharmaceutically acceptable salts thereof. In accordance with another aspect of this invention, there are provided novel intermediates, inter alia the novel compounds [6a] and [12a]. The novel intermediates of the present invention are stable, solid compounds, obtainable in high yields, which can be easily purified by crystallization and stored for long periods of time.

The invention relates to a method for producing anisidine by mixed nitrochlorobenzene (comprising o-nitrochlorobenzene, p-nitrochlorobenzene and m-nitrochlorobenzene) in an aqueous solvent through steps of etherification, hydrogenation, distillation separation, and the like. The method comprises the technical processes: (1) enabling the mixed nitrochlorobenzene and methanol to react, using water as a solvent and sodium hydroxide as a catalyst; (2) separating an aqueous phase; (3) catalyzing and hydrogenating etherified oil, and directly hydrogenating and reducing the etherified oil by using water as the solvent without washing to remove alkaline by water; (4) filtering the catalyst; (5) separating crude products, cooling and precipitating an organic phase, and separating and removing the water phrase; and (6) rectifying and separating an organic phase, and rectifying the organic phase obtained by separating water to obtain pure p-anisidine and pure o-anisidine with the purity over 99 percent. The method for producing anisidine by mixed nitrochlorobenzene reacting in an aqueous solvent has simple technology, low cost and energy consumption, high product purity, environmental protection and low toxicity.

The invention relates to a preparation method for p-anisidine. In the presence of a ternary amorphous alloy catalyst being Ni-Mo-B or Ni-Co-P, liquid-phase p-nitroanisole is subjected to hydrogenation through intermittent hydrogenation, and therefore p-anisidine with a selectivity of more than 99.7% can be obtained. In the preparation method, reaction conditions are mild, the solvent and the catalyst can be recycled, and the preparation method is liable to industrial production.

The invention discloses a method for preparing p-anisidine through catalytic hydrogenation of p-nitroanisole. According to the method, p-nitroanisole is used as a reaction raw material and subjected to a reaction in an enclosed reactor with a mechanical stirring function under the conditions of usage of a composite catalyst, no usage of a solvent, a reaction temperature of 80 to 150 DEG C and hydrogen pressure of 0.3 to 1 MPa so as to obtain p-anisidine, wherein the composite catalyst is composed of active components metal M and a carrier; the active components metal M are composed of two or more selected from a group consisting of Cu, Ni, Fe, Zn, Co, Cr and Mo, and the content of the active components metal M accounts for 0.3 to 25 wt% of the mass of the composite catalyst; and the carrier is prepared by compounding a carbon-containing organic matter and an inorganic oxide, a mass ratio of the carbon-containing organic matter to the inorganic oxide is 1: 50 to 1: 10, and the inorganicoxide is any one selected from a group consisting of SiO2, Al2O3, MgO, TiO2, CeO2 and a 4A molecular sieve. The composite catalyst used in the invention has high catalytic activity, stable performance and high selectivity and conversion rate.

The invention provides a method for preparing p-aminoanisole by hydrogenating p-nitroanisole. In the presence of KT-02 supported nickel catalyst, the reduction reaction of p-nitroanisole can be started under relatively mild conditions to generate p-aminoanisole. Compared with the existing techniques such as nitrobenzene method, sodium sulfide or iron reduction method, the present invention has the advantages of mild reaction conditions, fast reaction speed, clean reaction process, easy separation of products and the like.

The invention relates to a method of preparing o-anisidine and p-anisidine through hydrogenation reduction of a mixture of o-nitroanisole and p-nitroanisole. According to the method, o-nitroanisole and p-nitroanisole are used as raw materials, and o-anisidine and p-anisidine are prepared in a methanol system through hydrogenation reduction with Pt / C as a catalyst. With the method provided by the invention, the disadvantages of high energy consumption and high cost in conventional production process of o-anisidine and p-anisidine are overcome, and the technical problems of severe environmental pollution and loss of materials caused by considerable process waste water generated in the process of pretreatment in conventional production process are overcome; the method provided by the invention has the advantages of easiness, a high conversion rate, clean, green and environment-friendly process and a small amount of pollution by three wastes.

The invention relates a method for preparing p-anisidine through catalytic hydrogenation by an industrial-scale device. The method comprises the following steps: adding a raw material namely p-nitroanisole in an industrial-scale hydrogenation kettle in each production cycle in a continuous mode or an intermittent mode, and monitoring the concentrations of the raw material and impurities in the hydrogenation kettle in a reaction process in real time so as to obtain p-anisidine with the purity of 99.5% or above and yield of 100%. The purity of the p-anisidine product obtained through the method reaches 99.5% or above, so that p-anisidine can be directly used and sold; p-anisidine can further be subjected to rectification treatment to obtain a high-quality p-anisidine product with the purity of 99.9% or above which can be used in special fields.

The invention discloses a method for industrially synthesizing 4-chloro-3-nitroanisole from p-aminoanisole, which uses p-aminoanisole as a raw material, undergoes aminoacetylation protection, nitration, amino deprotection, Chlorination synthesized 4-chloro-3-nitroanisole. The preparation method of the present invention can be represented by the following reaction formula: ∴ M in the molecular formula e For methyl.

The invention discloses a detection method for soybean oil oxidation degree, belonging to detection technology for oil oxidation. The method comprises the following steps: (1) carrying out thermal oxidation treatment on soybean oil to obtain oxidized oil, then cooling the soybean oil and storing the soybean oil in cold atmosphere with temperature of -20 DEG C; (2) determining the conjugated diene value (CDV) and the p-anisidine value (p-AV) of the soybean oil and determining the proportion of fatty acid by utilizing gas chromatography; (3) carrying out correlation analysis between the conjugated diene value (CDV) as well as the p-anisidine value (p-AV) and the proportion of the fatty acid, and taking the proportion of the fatty acid with the correlation coefficient with the conjugated diene value (CDV) and the p-anisidine value (p-AV) greater than 0.9 as a parameter to represent the soybean oil oxidation degree. According to the method, by utilizing the intrinsic property of the composition of the oil fatty acid, the oil oxidation degree can be evaluated according to the proportion change, and therefore, the detection method is a convenient, accurate and quick detection method with low cost and strong reproducibility for the oil oxidation degree.

The invention discloses a preparation method of N-methyl-p-anisidine. The preparation method comprises the following steps: p-anisidine and methanol as reactants and a composite metal oxide A@B as a catalyst are subjected to a reaction in a fixed bed continuous flow reactor under conditions that reaction temperature is 200-350 DEG C, liquid volume space velocity is 0.1-2.0 h<-1> and N2 is used ascarrier gas, and N-methyl-p-anisidine is obtained; in the composite metal oxide A@B catalyst, A represents the active component CuO-ZnO-NiO or CuO-ZnO-Cr2O3, and B represents one of surface coatings Al2O3, SiO2 and TiO2 or C; the molar ratio of Cu to Zn is 0.1-10:1, the molar ratio of Cu to Ni is 0.1-10:1, and the molar ratio of Cu to Cr is 0.1-10:1; the surface coating Al2O3, SiO2 and TiO2 or C materials account for 1wt%-10wt% of the total amount of the catalyst. The method is simple to operate, and has the advantages of mild conditions, stable catalyst performance, high yield, low cost and low pollution.

Methods for the detection of spoilage of oils containing unsaturated fatty acids is disclosed. Specific methods include the determination of p-anisidine in oils containing unsaturated fatty acids using high performance liquid chromatography after p-an-isidine is added to the oil containing unsaturated fatty acids, and allowed to react with oxidation products.

The invention discloses a plastic material resistant to moisture environment. The plastic material comprises an outer layer and an inner layer. The outer layer covers the surface of the inner layer and wraps the inner layer inside. The inner layer contains a desiccant and the outer layer contains a colorant. The inner layer also contains plastic raw materials, the plastic raw materials are the following raw materials in parts by weight: 100-150 parts of polycarbonate, 30-50 parts of ABS plastics, 5-10 parts of epoxy resin, 5 parts of ethylene bis stearamide ‑8 parts, 10‑15 parts of mercapto acrylate, 5‑10 parts of N‑cyclohexyl p-methoxyaniline, 17‑20 parts of polyethylene, 3‑7 parts of color masterbatch, 10‑12 parts of styrene‑butylene and titanium 4-8 parts of acid ester. The invention adopts a double-layer material design, which can provide good moisture-proof effect.

The invention discloses a quality control material for metabolomics detection and a quality control method of the quality control material. The quality control material comprises mixed standard samples of 4,4'-methylene bis(2-chloroaniline), p-anisidine, L-tyrosine methyl ester, 3-chloroaniline, 2,4-dimethyl quinoline, sulfapyridine, atrazine, sulfadoxine, DL-leucine, N-benzoyl-L-tyrosine ethyl ester, 6-phenyl-2-thiouracil, N-(o-toluoyl) glycine, 2-methyl-5-nitroimidazole-1-ethanol, glycyrrhetinic acid, flavanone, Epsilon-caprolactone and 2-aminopyridine. 17 standard samples in the method comefrom different material categories and are very stable, simple in preparation and small in amount; and the quality control material disclosed by the invention can accurately reflect the state of a chromatograph or a mass spectrometer.

The invention provides a polyurethane material with an electrochromic property as well as a preparation method and application of the polyurethane material, relates to the polyurethane material with the electrochromic property and the preparation method of the polyurethane material, and aims to solve the problems that common polyurethane is not liable to dissolve and difficult to process and does not have the electrochromic property. The preparation method comprises the following steps: I, adding p-Anisidine and 1-fluoro-4-nitrobenzene into a dimethyl sulfoxide solvent, and performing a reaction so as to prepare methoxyl dinitro triphenylamine; II, reducing the methoxyl dinitro triphenylamine, so as to obtain diamino triphenylamine; III, preparing isocyanate; IV, adding the isocyanate and an aromatic bisphenol monomer into dimethyl formamide, and preparing polyurethane; V, performing drying so as to obtain a polyurethane film. The polyurethane material is applied in such a way that a gel electrolytic solution is applied between the polyurethane film and an ion storing layer, and after encapsulation is performed, a polyurethane device with the electrochromic property is obtained. According to the polyurethane material, as well as the preparation method and the application thereof disclosed by the invention, triphenylamine is introduced into the polyurethane material, so that the processing solubility and the reversible electrochromic property of the polyurethane are realized.

The present invention provides a method for aqueous enzymatic extraction of soybean oil, which is in the field of extraction processing technology for plant oil. The method comprises treating crushed and peeled soybeans with an extrusion puffing process and a hydrolysis process with an alkaline proteinase, followed by a liquid nitrogen freezing and a high voltage electrostatic thawing process, and finally obtaining soybean oil by centrifugation. The benefits of the present invention includes short extraction time and high extraction yield. It saves up to 93.1% of time in the freezing and thawing process alone. The total oil yield is up to 95.4%. Furthermore, the method of the invention produces high quality oil with a low peroxide value, a low p-anisidine value and a low TOTOX value.

The invention discloses a nitrogen heterocyclic butanone and belongs to the technical field of heterocyclic compounds. The nitrogen heterocyclic butanone is chemically named as (3S,4S)-3-[(1R)-hydroxy ethyl]-4-benzene acetyl-1-p-methoxyphenyl-2-nitrogen heterocyclic butanone (compound I). A synthesis method comprises the following steps: (1) the synthesis of a compound II, namely performing a reaction on L-threonine and p-anisidine under the action of CDI (Carbon Dioxide Ice) by taking ethyl acetate as a solvent; (2) the synthesis of a compound III, namely performing an epoxidation reaction on the compound II with HCl, NaNO2 and NaOH; (3) the synthesis of a compound IV, namely performing the reaction on the compound III and 2-chloroethene benzophenone so as to synthesize the compound IV; (4) the synthesis of the compound I, namely performing a cyclization reaction on the compound IV under the action of zinc chloride and piperidine so as to synthesize the compound I. The method is high in reaction yield; the selectivity of the reactions is improved and the epoxide butyrylamide is almost all converted into a target product by taking the zinc chloride as a lewis acid.

The invention relates to a method for producing anisidine by mixed nitrochlorobenzene (comprising o-nitrochlorobenzene, p-nitrochlorobenzene and m-nitrochlorobenzene) in an aqueous solvent through steps of etherification, hydrogenation, distillation separation, and the like. The method comprises the technical processes: (1) enabling the mixed nitrochlorobenzene and methanol to react, using water as a solvent and sodium hydroxide as a catalyst; (2) separating an aqueous phase; (3) catalyzing and hydrogenating etherified oil, and directly hydrogenating and reducing the etherified oil by using water as the solvent without washing to remove alkaline by water; (4) filtering the catalyst; (5) separating crude products, cooling and precipitating an organic phase, and separating and removing the water phrase; and (6) rectifying and separating an organic phase, and rectifying the organic phase obtained by separating water to obtain pure p-anisidine and pure o-anisidine with the purity over 99 percent. The method for producing anisidine by mixed nitrochlorobenzene reacting in an aqueous solvent has simple technology, low cost and energy consumption, high product purity, environmental protection and low toxicity.

The invention discloses a clean production method of p-anisidine. The clean production method comprises the following steps of (1) enabling nitrochlorobenzene, sodium hydroxide and methanol to be subjected to an etherification reaction so as to obtain etherification reaction liquid; (2) directly filtering the etherification reaction liquid obtained in the step (1) to obtain a filtrate and filter cakes, washing the filter cakes with the methanol, drying the washed filter cakes to obtain industrial-grade sodium chloride, and distilling the filtrate so as to obtain p-nitroanisole concentration liquid; and (3) under the condition that a hydrogenation catalyst exists, enabling the p-nitroanisole concentration liquid obtained in the step (2) to be subjected to a hydrogenation reduction reaction in the hydrogen atmosphere, and after the reaction is completed, performing after-treatment so as to obtain the p-anisidine. According to the clean production method, after the etherification reaction is finished, direction filtration is performed so that the sodium chloride is removed, then concentration treatment is performed on the etherification reaction liquid, the hydrogenation reaction is directly performed, the operation is simple and convenient, and the yield and the purity of the obtained product are high.

The invention relates to a preparation method of 2'-[bis (phenylmethyl) amino]-6'-(diethylamino)-spiro [isobenzofuran-1 (3H), 9'-[9H] xanthen]-3-one. The preparation method comprises the steps of conducting condensation reaction in fuming sulfuric acid by using 2-(hydroxyl-4-diethylamino-2-hydroxybenzoyl) benzoic acid and N, N-diphenylmethyl-p-anisidine, then adding water and methylbenzene, conducting extraction and layering, removing an acid water layer, adding alkali, conducting cyclization reaction, conducting heating and distillation to remove methylbenzene, finally adding methanol for refining and conducting vacuum drying to obtain GREEN refined products. The preparation method has the advantages that since catalysts are added, the reaction yield of 2-(hydroxyl-4-diethylamino-2-hydroxybenzoyl) benzoic acid is improved to 98 percent; since the fuming sulfuric acid is used to replace concentrated sulfuric acid, the amount of generated sulfonate is reduced; and since alkalinity pH (potential of hydrogen) is controlled to be less than 12, the appearance characteristic and the yield of the products are improved and the product yield is improved to more than 82 percent.

The invention discloses a method for synthesizing biaryl hydrocarbons, which belongs to the field of organic catalytic synthesis. Using poly-p-methoxyaniline-loaded nano-palladium as a catalyst and diisopropylethylamine as a base in N-methylpyrrolidone solvent, hydrazine hydrate is used to catalyze the reduction of halogenated hydrocarbons to prepare biaryls. The reaction conditions of the present invention are mild, the product is easy to separate, the reaction is easy to operate, and has good safety; secondly, the catalyst used in the method is easy to prepare, the amount is small, and the catalyst can be recycled many times after the reaction; in addition, the present invention uses Green alkali and reducing agent, less solid waste, low corrosion, green and environmentally friendly.

The invention discloses a method for detecting the residual quantity of aminoanisole and paranitroanisole in soil and belongs to the field of analysis and detection. The method comprises the steps of sample preparation, thermal desorption-gas chromatograph-mass spectrometer measurement, and external standard method quantification. The method is suitable for measuring the residual quantity of aminoanisole and paranitroanisole in soil and is simple, convenient to use and environmentally friendly, detection limit is low, and accuracy is high.

The invention provides a polyurethane material with an electrochromic property as well as a preparation method and application of the polyurethane material, relates to the polyurethane material with the electrochromic property and the preparation method of the polyurethane material, and aims to solve the problems that common polyurethane is not liable to dissolve and difficult to process and does not have the electrochromic property. The preparation method comprises the following steps: I, adding p-Anisidine and 1-fluoro-4-nitrobenzene into a dimethyl sulfoxide solvent, and performing a reaction so as to prepare methoxyl dinitro triphenylamine; II, reducing the methoxyl dinitro triphenylamine, so as to obtain diamino triphenylamine; III, preparing isocyanate; IV, adding the isocyanate and an aromatic bisphenol monomer into dimethyl formamide, and preparing polyurethane; V, performing drying so as to obtain a polyurethane film. The polyurethane material is applied in such a way that a gel electrolytic solution is applied between the polyurethane film and an ion storing layer, and after encapsulation is performed, a polyurethane device with the electrochromic property is obtained. According to the polyurethane material, as well as the preparation method and the application thereof disclosed by the invention, triphenylamine is introduced into the polyurethane material, so that the processing solubility and the reversible electrochromic property of the polyurethane are realized.

The invention discloses a synthesis method of a bazedoxifene derivative. According to the preparing method of the bazedoxifene derivative, p-anisidine is adopted as a raw material, and through a six-step reaction, the synthesis of the bazedoxifene derivative is achieved. The preparing method of the bazedoxifene derivative is reasonable in technological design and high in operability, the reaction condition is mild, the yield is high, and thus industrialized production can be achieved. The prepared bazedoxifene derivativ bazedoxifene provides an important basis for scientific evaluation of quality, safety and efficiency of bazedoxifene; meanwhile, the bazedoxifene derivative is good in pharmacological activity, can be developed into medicines used for treating osteoporosis, and thus the bazedoxifene derivative has important application value.

The invention provides a method for synthesizing biaryl and belongs to the field of organic catalytic synthesis. Poly p-anisidine loaded nano-palladium serves as a catalyst, diisopropylethylamine serves as an alkali, in a N-methyl pyrrolidinone solvent, and the reduction of halohyrocarbons with hydrazine hydrate is catalyzed to prepare biaryl. According to the method, the reaction condition is mild, products are easy to separate, the reaction is easy to operate, and good safety is achieved. Secondly, the catalyst used in the method is easy to prepare, the use amount is small, and after the reaction is completed, the catalyst can be recycled for many times. In addition, in the method, the green alkali and the green reduction agent are used, solid waste is little, corrosivity is low, and the method is green and environmentally friendly, and protects the environment.

The invention relates to the field of oil extraction, and discloses a deodorization method for improving the quality of microalgae oil rich in DHA (docosahexaenoic acid). The deodorization method comprises the following steps: firstly, fermenting DHA through schizophyllum commune, then carrying out cell lysis and centrifugation to obtain DHA-rich oil, and carrying out pre-refining to obtain decolored oil. And carrying out deodorization treatment on the decolorized oil, heating ionized water used for deodorization until the ionized water is boiled, discharging gas and steam separated from the water, and then pumping the gas and the steam into a steam generator. And the pre-deoxygenated water is further heated to form steam. And then deodorization is carried out. According to the method, the peroxide value and p-anisidine value of the grease are effectively reduced by reducing the negative influence of oxygen, and finally a high-quality product meeting market requirements is obtained.

The invention discloses a nitrogen heterocyclic butanone and belongs to the technical field of heterocyclic compounds. The nitrogen heterocyclic butanone is chemically named as (3S,4S)-3-[(1R)-hydroxy ethyl]-4-benzene acetyl-1-p-methoxyphenyl-2-nitrogen heterocyclic butanone (compound I). A synthesis method comprises the following steps: (1) the synthesis of a compound II, namely performing a reaction on L-threonine and p-anisidine under the action of CDI (Carbon Dioxide Ice) by taking ethyl acetate as a solvent; (2) the synthesis of a compound III, namely performing an epoxidation reaction on the compound II with HCl, NaNO2 and NaOH; (3) the synthesis of a compound IV, namely performing the reaction on the compound III and 2-chloroethene benzophenone so as to synthesize the compound IV; (4) the synthesis of the compound I, namely performing a cyclization reaction on the compound IV under the action of zinc chloride and piperidine so as to synthesize the compound I. The method is high in reaction yield; the selectivity of the reactions is improved and the epoxide butyrylamide is almost all converted into a target product by taking the zinc chloride as a lewis acid.

The invention discloses a universal quality control product and a quality control method for metabonomics detection. The universal quality control product comprises a mixed standard sample of 4,4'-methylene bis(2-chloroaniline), p-anisidine, L-tyrosine methyl ester, 3-chloroaniline, 2, 4-dimethyl quinoline, sulfadiazine, atrazine, sulfadoxine, DL-leucine, N-benzoyl-L-tyrosine ethyl ester, 6-phenyl-2-thiouracil, N-(o-toluoyl) glycine, 2-methyl-5-nitroimidazole-1-ethanol, glycyrrhetinic acid, flavanone, epsilon-caprolactone and 2-aminopyridine. The 17 standard samples are derived from differentsubstance types, and are very stable, simple to prepare and small in usage amount. The quality control product can accurately reflect an instrument state of a chromatographic instrument or a mass spectrometer, and can successfully analyze instable reasons according to a spectrogram overlapping situation; and the judging accuracy reaches 100%.