- Synthesis method of high-purity 2 - nitro -4-aminoanisole
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The invention discloses a synthesis method of high-purity 2 -nitro -4-aminoanisole, wherein 2 - nitro -4-n-aminoanisole is synthesized through an assembly line. The assembly line comprises a reaction device, a discharging device and a cleaning device. The method comprises the following steps: A, feeding reaction raw materials into a reaction device for reaction. B, Use clear bottom device to carry out the stirring to phase transfer catalyst and reaction raw materials. C, Use the cleaning device to clean the bottom of reation kettle. D, The extrusion device is used to clean and blow the cleaning device and the bottom cleaning device, and the catalyst and the reaction raw material are pushed up and down. E: The extraction bucket is used to extract the product in the reaction liquid and the extracted reaction is continued to return to the reaction kettle. F, Use the discharging device to make the reaction all discharge. G, Wash the reaction liquid with the cleaning device, obtain the finished product.
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Paragraph 0057-0062
(2021/11/19)
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- A 2 - amino - 4 - acetyl amino methyl ether synthesis method (by machine translation)
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The invention discloses a 2 - amino - 4 - acetyl amino methyl ether synthesis method. The synthetic method comprises the following steps: (1) in the presence of a catalyst A, to nitroanisole with hydrogen by a catalytic hydrogenation reduction reaction to obtain the amino anisole; (2) P a the fuel to the acetylation reaction acetyl amino anisole; (3) to the acetaminophen a fuel for nitration reaction to obtain the 2 - nitro - 4 - acetamido anisole; (4) in the presence of a catalyst B, 2 - nitro - 4 - acetyl amino methyl ether with hydrogen by secondary catalytic hydrogenation reduction reaction. This invention adopts the first acylation, re-nitration, reduction method for synthesis of 2 - amino - 4 - acetyl amino methyl ether, avoids the traditional directional acylate raw material is easy to oxidation in the process, a plurality of side reaction, the product is hard to separate, the problem of low purity, the method of the invention the synthetic product purity can be up to 99.5% -99.8%. (by machine translation)
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Paragraph 0069; 0070
(2018/05/01)
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- Industrial production method for 2-amino-4-acetamidoanisole
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The invention discloses an industrial production method for 2-amino-4-acetamidoanisole. The industrial production method comprises the following steps: (1) allowing paranitroanisole and hydrogen to undergo a catalytic hydrogenation reduction reaction in the presence of a catalyst A so as to obtain p-aminoanisole; (2) allowing the p-aminoanisole to undergo an acetylation reaction so as to obtain p-acetamidoanisole; (3) allowing the p-acetamidoanisole to undergo a nitration reaction so as to obtain 2-nitro-4-acetamidoanisole; and (4) allowing 2-nitro-4-acetamidoanisole and hydrogen to undergo two catalytic hydrogenation reduction reactions in the presence of a catalyst B so as to obtain the 2-amino-4-acetamidoanisole. The production method provided by the invention has the characteristics oflow production cost, high reaction selectivity, simple separation process, high product purity, no three wastes in the process of production, recyclability and continuous large-scale industrial production, and solves the disadvantages of high separation cost, low product purity, and large discharge amount and difficult treatment of three wastes in the prior art.
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Paragraph 0055; 0060
(2018/04/03)
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- 2 - Amino - 4 - acetamido anisole novel synthesis process (by machine translation)
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The present invention provides a novel 2 - amino - 4 - acetamido anisole synthesis process, the usage of palladium bi-metal catalysts and the palladium/carbon catalyst to replace Rany - Ni catalyst, to the anisole on the nitro-selective catalytic hydrogenation, which not only reduces use Rany - Ni catalyst of post-industrial risks, while at the same time, the resulting 2 - amino - 4 - acetyl anisole purity higher, greater yield. (by machine translation)
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- Synthesis process of 2-amidogen-4-acetamido anisole
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The invention discloses a synthesis process of 2-amidogen-4-acetamido anisole. The synthesis process of the 2-amidogen-4-acetamido anisole comprises the steps of adopting p-methoxyaniline as a raw material, carrying out partial acylation reaction on the p-methoxyaniline and acetic anhydride, and preparing to obtain p-acetamido anisole; then carrying out nitration reaction, carrying out one-pot method'reaction to obtain 2-nitro-4-acetamido anisole, and under the action of a Pd/C catalyst, reducing the 2-nitro-4-acetamido anisole by adopting hydrazine monoformate as a hydrogen source to preparethe 2-amidogen-4-acetamido anisole. The synthesis process provided by the invention is low in energy consumption, low in cost, less in solid wastes and waste liquids, green and environmentally friendly, simple to operate, mild in reaction conditions, and high in industrial safety coefficient, the total yield of the target compound is 85 percent or above (on the basis of an initial reaction raw material), the HPLC (High Performance Liquid Chromatography) purity is 99.0 percent or above, the target compound is high in yield and good in quality, and the synthesis process is more suitable for industrial production.
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Paragraph 0042-0043; 0046-0047; 0049-0050; 0052-0053
(2020/03/28)
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- Regioselective nitration of anilines with Fe(NO3)3·9H2O as a promoter and a nitro source
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An efficient Fe(NO3)3·9H2O promoted ortho-nitration reaction of aniline derivatives has been developed. This reaction may go through a nitrogen dioxide radical (NO2) intermediate, which is generated by the thermal decomposition of iron(iii) nitrate. The practicality of the present method using nontoxic and inexpensive iron reagents has been shown by the broad substrate scope and applications.
- Gao, Yang,Mao, Yuanyou,Zhang, Biwei,Zhan, Yingying,Huo, Yanping
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supporting information
p. 3881 - 3884
(2018/06/08)
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- Preparation method of 2-nitro-4-acetamidoanisole
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The invention discloses a preparation method of 2-nitro-4-acetamidoanisole. The preparation method comprises the following step: under the action of concentrated sulfuric acid, performing nitration reaction as shown below on a compound as shown in a formula 4 and an aqueous nitric acid solution having the mass fraction of 30-80% to obtain a compound as shown in a formula 5, wherein the percent of the 30-80% aqueous nitric acid solution is the mass percent of the nitric acid in the aqueous nitric acid solution. The preparation method is high in safety, free of special equipment requirement and environment-friendly, and is suitable for industrial production.
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Paragraph 0105; 0106; 0111-0114
(2017/11/04)
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- Disperse dye intermediate preparation method
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The invention provides a disperse dye intermediate preparation method, which is characterized by utilizing m-dinitrobenzene as a raw material and obtaining a target product through amination, amidation and reduction reaction. In addition, the disperse dye intermediate preparation method disclosed by the invention enables waste residues generated in a reaction process to be recycled through a circular metal reduction method. Furthermore, the disperse dye intermediate preparation method disclosed by the invention has environmental friendliness and no pollution.
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Paragraph 0076; 0078
(2017/08/31)
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- Preparation method of 2-methoxy-5-acetamidoaniline
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The invention discloses a preparation method of 2-methoxy-5-acetamidoaniline. The preparation method comprises the following step: in a solvent, under the action of a catalyst Pd/C, performing a reduction reaction as shown below on a compound as shown in a formula 5 and hydrogen to obtain a compound as shown in a formula 6. The preparation method is low in pollution, high in yield rate, low in cost, convenient in catalyst or solvent recycling, short in reaction time, low in reaction temperature, high in safety and mild in reaction condition.
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- Method for recovering 2,4-dinitrophenol hydrogenation reduction byproduct to prepare 2-amino-4-acetamidoanisole
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The invention discloses a method for recovering 2,4-dinitrophenol hydrogenation reduction byproduct to prepare 2-amino-4-acetamidoanisole. The method comprises the following steps: separating a 2-amino-4-nitrophenol and 2-nitro-4-aminophenol mixture to obtain a 2-nitro-4-aminophenol single component; mixing the 2-nitro-4-aminophenol with an alkylation reagent, and carrying out a phenolic hydroxyl group alkylation reaction and an amino group acylation reaction to obtain 2-nitro-4-acetamidoanisole; and carrying out nitro group reduction on the 2-nitro-4-acetamidoanisole to obtain the 2-amino-4-acetamidoanisole. The method provides a brand new method for the synthesis of the fine chemical engineering intermediate 2-amino-4-acetamidoanisole with important uses, reduces the content of organic matters in 2-amino-4-nitrophenol production wastewater, reduces the treatment difficulty of enterprises' industrial wastewater, converts wastewater components into the fine chemical engineering intermediate with important production uses, and increases the enterprises' economy income.
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Paragraph 0024-0027
(2017/07/22)
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- The novel usage of thiourea nitrate in aryl nitration
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Thiourea nitrate (TN) was easily prepared from thiourea and nitric acid to explore its use as a new nitration reagent. Nitrations of various aromatic compounds utilizing TN in concentrated sulfuric acid were studied. TN could convert aromatic compounds to the corresponding nitrated derivatives with various abnormal yields under mild conditions. The results suggested that the reaction mechanism might be different from those of traditional nitration reagents.
- Meng, Ge,Zheng, Mei-Lin,Zheng, A-Qun,Wang, Mei,Shi, Juan
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- Functionalized alkoxy arene diazonium salts from paracetamol
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Arene diazonium tetrafluoroborates can be synthesized from aromatic acetamides via a sequence of deacetylation, diazotation and precipitation, induced by anion exchange. The reaction is conducted as a convenient one-flask transformation with consecutive addition of the appropriate reagents. Exchange of solvents or removal of byproducts prior to isolation of the product is not required. The arene diazonium salts are isolated from the reaction mixture by simple filtration. Two complementary protocols are presented, and the utility of the reaction is exemplified for a synthesis of the diarylheptanoid natural product de-O-methyl centrolobine.
- Schmidt, Bernd,Berger, Rene,Hoelter, Frank
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supporting information; experimental part
p. 1406 - 1414
(2010/06/19)
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- Guanidinium nitrate: A novel reagent for aryl nitrations
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Nitration of various aromatic compounds utilising guanidinium nitrate in 85% sulfuric acid as a nitrating agent has been studied.
- Ramana,Malik,Parihar
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p. 8681 - 8683
(2007/10/03)
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- Process for preparing free-flowing 2-nitro-4-acetylamino-anisole
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2-Nitro-4-acetylamino-anisole is prepared directly in the form of a moist, free-flowing material by nitrating 4-acetylamino-anisole and then treating the reaction mixture with water at slightly elevated temperatures, e.g., 20-60° C.
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