93-26-5Relevant articles and documents
A Mild Heteroatom (O -, N -, and S -) Methylation Protocol Using Trimethyl Phosphate (TMP)-Ca(OH) 2Combination
Tang, Yu,Yu, Biao
, (2022/03/27)
A mild heteroatom methylation protocol using trimethyl phosphate (TMP)-Ca(OH)2combination has been developed, which proceeds in DMF, or water, or under neat conditions, at 80 °C or at room temperature. A series of O-, N-, and S-nucleophiles, including phenols, sulfonamides, N-heterocycles, such as 9H-carbazole, indole derivatives, and 1,8-naphthalimide, and aryl/alkyl thiols, are suitable substrates for this protocol. The high efficiency, operational simplicity, scalability, cost-efficiency, and environmentally friendly nature of this protocol make it an attractive alternative to the conventional base-promoted heteroatom methylation procedures.
Continuous synthesis method 2 -acetylamino -5 - nitroanisole
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Paragraph 0035, (2021/11/03)
The invention mainly relates to the field of organic synthesis, and discloses a continuous synthesis process for 2 -acetylamino -5 - nitroanisole. The process takes a microchannel continuous flow reactor as a main reaction device, and anthranilic acid is taken as a starting raw material and is subjected to preacylation. And nitration, a continuous synthesis 2 - acetylamino -5 - nitroanisole was achieved. To the process, the compound amidation reagent is adopted, the raw material cost is reduced, and the amidation reagent and the reaction solvent are unified. The continuous production process and equipment are introduced, continuous production is realized, the automation degree is improved, and the production safety risk is greatly reduced. The reaction time, the generation of by-products and the subsequent treatment difficulty are reduced, the nitration selectivity is improved, the economic benefits and environmental benefits are achieved, and the development concept of the green chemistry is met.
Visible-light induced one-pot hydrogenation and amidation of nitroaromatics with carboxylic acids over 2D MXene-derived Pt/N-TiO2/Ti3C2
Jiang, Heyan,Hu, Zujie,Gan, Chuan,Sun, Bin,Kong, Shuzhen,Bian, Fengxia
, (2021/03/03)
Pt nanoparticles supported on N doped titanium dioxide/titanium carbide (MXene) heterojunctions were employed as photocatalysts for the tandem reactions between aromatic nitro compounds and carboxylic acids to produce amide products. The 3%Pt/N-TiO2/Ti3C2 heterojunction was prepared by in situ grew TiO2 on Ti3C2 nanosheets and then N doped TiO2 with melamine, Pt nanoparticles with 3.3 nm mean diameter well dispersed on N-TiO2/Ti3C2. 3%Pt/N-TiO2/Ti3C2 had excellent amidation activity and chemoselectivity under visible-light irradiation. The elevated catalytic performance of 3%Pt/N-TiO2/Ti3C2 was owing to the improvement in photogenerated electron and hole separation efficiency through charge short-range directional transmission caused by the intimate contact between the TiO2 and the conductive Ti3C2. This direct hydrogenation along with amidation between nitroaromatics and carboxylic acids own actual merits in the amides produce with no harmful byproducts. In situ DRIFTS spectra verified that the amidation activation with visible light irradiation at 25 °C was much faster than heating.
