- Method for preparing 3, 4'-diaminodiphenyl ether
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The invention discloses a method for preparing 3, 4'-diaminodiphenyl ether, which mainly comprises the following steps: adding m-aminophenol, an acid-binding agent and a solvent into a condensation reaction kettle, stirring, heating under the protection of inert gas, keeping the temperature at 100-120 DEG C, dropwisely adding p-nitrochlorobenzene, keeping the temperature for 2-4 hours after 5-7 hours, and continuing the reaction; after the reaction is finished, filtering to remove inorganic salt, transferring a filtrate into a hydrogenation kettle, adding a noble metal catalyst and a cocatalyst, performing nitrogen replacement, maintaining the temperature at 60-80 DEG C, and introducing hydrogen for catalytic hydrogenation under the hydrogen pressure of not more than 0.5 MPa; after the reaction is finished, filtering out the catalyst, distilling the filtrate, removing the solvent, rectifying, collecting 206-210 DEG C (2-3 mmHg) fraction which is white 3, 4'-diaminodiphenyl ether, and packaging under the protection of nitrogen. The method is short in process step, low in energy consumption and low in production cost, the content of the obtained 3, 4'-diaminodiphenyl ether is largerthan 99.5%, and the total molar yield is larger than 93%.
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Paragraph 0026-0032
(2020/05/14)
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- Fine-Bubble-Based Strategy for the Palladium-Catalyzed Hydrogenation of Nitro Groups: Measurement of Ultrafine Bubbles in Organic Solvents
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Fine bubbles of hydrogen were employed as a new reaction medium for the autoclave-free gas-liquid-solid multiphase hydrogenation of nitro groups on a multigram scale. Furthermore, ultrafine bubbles were examined by nanoparticle-tracking analysis in organic solvents.
- Mase, Nobuyuki,Nishina, Yuki,Isomura, Shogo,Sato, Kohei,Narumi, Tetsuo,Watanabe, Naoharu
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supporting information
p. 2184 - 2188
(2017/09/26)
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- Orthogonal Cu- and Pd-based catalyst systems for the O- and N-arylation of aminophenols
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O- or N-arylated aminophenol products constitute a common structural motif in various potentially useful therapeutic agents and/or drug candidates. We have developed a complementary set of Cu- and Pd-based catalyst systems for the selective O- and N-arylation of unprotected aminophenols using aryl halides. Selective O-arylation of 3- and 4-aminophenols is achieved with copper-catalyzed methods employing picolinic acid or CyDMEDA, trans-N,N′-dimethyl-1,2- cyclohexanediamine, respectively, as the ligand. The selective formation of N-arylated products of 3- and 4-aminophenols can be obtained with BrettPhos precatalyst, a biarylmonophosphine-based palladium catalyst. 2-Aminophenol can be selectively N-arylated with CuI, although no system for the selective O-arylation could be found. Coupling partners with diverse electronic properties and a variety of functional groups can be selectively transformed under these conditions.
- Maiti, Debabrata,Buchwald, Stephen L.
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supporting information; experimental part
p. 17423 - 17429
(2010/03/25)
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- Functionalized Photoreactive Compounds
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The present invention concerns functionalized photoreactive compounds of formula (I), that are particularly useful in materials for the alignment of liquid crystals. Due to the adjunction of an electron withdrawing group to specific molecular systems bearing an unsaturation directly attached to two unsaturated ring systems, exceptionally high photosensitivities, excellent alignment properties as well as good mechanical robustness could be achieved in materials comprising said functionalized photoreactive compounds of the invention.
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- Thermoplastic resin composition and a method of molding the same
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This invention provides a thermoplastic resin composition comprising a thermoplastic resin and 0.1 to 100 parts by weight, per 100 parts by weight of the thermoplastic resin, of an imide compound prepared, e.g., by dehydration condensation of 1,2,3,4-butanetetracarboxylic acid or a monoanhydride or a dianhydride thereof with a primary amine, and a method of molding the resin composition.
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- Method for the manufacture of 3-aminophenol
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A method of dehydrogenating 3-amino-2-cyclohexene-1-one with a supported palladium or palladium-platinum catalyst in a solvent in the presence of base to produce 3-aminophenol and its use directly without purification to produce 3,4'-oxydianiline.
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