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
Ru-Catalyzed Deoxygenative Transfer Hydrogenation of Amides to Amines with Formic Acid/Triethylamine
Pan, Yixiao,Luo, Zhenli,Xu, Xin,Zhao, Haoqiang,Han, Jiahong,Xu, Lijin,Fan, Qinghua,Xiao, Jianliang
supporting information, p. 3800 - 3806 (2019/07/12)
A ruthenium(II)-catalyzed deoxygenative transfer hydrogenation of amides to amines using HCO2H/NEt3 as the reducing agent is reported for the first time. The catalyst system consisting of [Ru(2-methylallyl)2(COD)], 1,1,1-tris(diphenylphosphinomethyl) ethane (triphos) and Bis(trifluoromethane sulfonimide) (HNTf2) performed well for deoxygenative reduction of various secondary and tertiary amides into the corresponding amines in high yields with excellent selectivities, and exhibits high tolerance toward functional groups including those that are reduction-sensitive. The choice of hydrogen source and acid co-catalyst is critical for catalysis. Mechanistic studies suggest that the reductive amination of the in situ generated alcohol and amine via borrowing hydrogen is the dominant pathway. (Figure presented.).
