94-68-8Relevant articles and documents
Production process of alkaline red intermediate 3-ethylamino-p-methylphenol
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Paragraph 0060-0062, (2021/03/31)
The invention relates to a production process of an alkaline red intermediate 3-ethylamino p-methylphenol. The production process specifically comprises the following steps: step 1, an alkylation reaction: carrying out alkylation reaction on o-toluidine and absolute ethyl alcohol under the action of a catalyst magnetic solid acid to generate an alkylate mixture; and then rectifying the alkylate mixture to obtain the N-ethyl o-toluidine; wherein the reaction temperature of the alkylation reaction is 60-120 DEG C; wherein the addition amount of the magnetic solid acid is 4-6% of the mass ratio of the feed liquid; step 2, a sulfonation reaction: carrying out sulfonation reaction on the N-ethyl o-toluidine and fuming sulfuric acid to generate 3ethylamino-p-toluenesulfonic acid; step 3, a hydroxylation reaction: carrying out hydroxylation reaction on 3ethylamino p-toluenesulfonic acid and potassium hydroxide to generate 3-ethylamino p-methylphenol potassium salt; and step 4, acid precipitation: reacting the 3-ethylamino p-methylphenol potassium salt with hydrochloric acid to prepare the 3-ethylamino p-methylphenol. The production process is high in yield and short in reaction time.
Homogeneous cobalt-catalyzed deoxygenative hydrogenation of amides to amines
Papa, Veronica,Cabrero-Antonino, Jose R.,Spannenberg, Anke,Junge, Kathrin,Beller, Matthias
, p. 6116 - 6128 (2020/11/03)
The first general and efficient cobalt-catalyzed deoxygenative hydrogenation of amides to amines is presented. The optimal catalytic system based on a combination of [Co(NTf2)2] and (p-anisyl)triphos (L3) in the presence of [Me3SiOTf] as acidic co-catalyst facilitates the direct hydrogenation of a broad range of amides to the corresponding amines under mild conditions. A set of control experiments indicate that, after the initial reduction of the amide carboxylic group to the well-known hemiaminal intermediate, the reaction mainly proceeds through C-O bond cleavage though other pathways might be also involved to a minor extent. This journal is
Alkylation of Aromatic Amines with Trialkyl Amines Catalyzed by a Defined Iridium Complex with a 2-Hydroxypyridylmethylene Fragment
Deng, Danfeng,Hu, Bowen,Zhang, Ziyu,Mo, Shengkai,Yang, Min,Chen, Dafa
, p. 2218 - 2226 (2019/05/21)
Six Cp?Ir complexes containing NN-bitentate chelate ligands [Cp?IrCl(C5H4CH2C5H3OH)][Cl] (1), [Cp?IrCl(C5H4CH2C5H3O)] (2), [Cp?IrCl(C5H4C5H3OH)] [Cl] (3), [Cp?IrCl(C5H4CH2C5H4)][Cl] (4), [Cp?IrCl(CH3OC5H3CH2C5H3OCH3)][Cl] (5), and [Cp?IrCl(CH3OC5H3CH2C5H3OH)][Cl] (6) were synthesized and characterized. Complex 1 could be transformed to 2 when reacted with NaOtBu or NEt3 via -OH deprotonation. These six complexes were tested as catalysts for mono-N-alkylation of amines with trialkyl amines, and complex 1 exhibited highest activity. The coupling reactions proceed under air condition, with 1 mol % catalyst loading without extra base in methanol at 120 °C and can be further accelerated by adding NR3·HCl.