2447-79-2Relevant articles and documents
Half-sandwich Ruthenium(II) Schiff base complexes: Synthesis, characterization and effective catalysts for one-pot conversion of aldehydes to amides
Premkumar, Muniyappan,Vijayan, Paranthaman,Venkatachalam, Galmari
, (2019)
Five new Schiff base ligands and conformationally rigid half-sandwich organo ruthenium(II) Schiff base complexes (1–5) with the general formula [Ru(η6?p?cymene)(Cl)(L1-5)] (where, L = mono anionic Schiff base ligands) have been synthesized from the reaction of [{(η6?p?cymene)RuCl}2(μ?Cl)2] with a bidentate Schiff bases ligands. These ruthenium(II) Schiff base complexes were fully characterized by elemental analysis, FT?IR, UV–Vis, 1H & 13C NMR and mass spectroscopy studies. In chloroform solution, all the metal complexes exhibit characteristic metal to ligand charge transfer bands (MLCT) and emission bands in the visible region. The crystal structure of the complexes [Ru(η6?p?cymene)(Cl)(L1)] (1) and [Ru(η6?p?cymene)(Cl)(L3)] (3) were determined by single crystal X?ray crystallography. The complexes exhibited good catalytic activity for aldehydes to amides by one-pot conversion process in the presence of NaHCO3/NH2OH·HCl.
Method for efficient solid-phase synthesis of amide derivative through carboxylic acid and urea
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Paragraph 0022-0030, (2019/11/12)
The invention discloses a method for efficient solid-phase synthesis of an amide derivative through carboxylic acid and urea. The method comprises the steps that a carboxylic acid and urea mixture anda catalyst are mixed, a mixture is placed in a sealed pipe of a single-mode microwave device and heated, then through a monitoring reaction endpoint, namely the ratio, being 4:1, of cyclohexane to ethyl acetate in thin-layer chromatography (TLC), reactants are cooled to the room temperature, extraction is conducted through the ethyl acetate, then an extract is sequentially washed by hydrochloricacid, a sodium bicarbonate solution and water, an organic layer is dried by anhydrous magnesium sulfate, a solvent is subjected to decompressed distillation, and thus the amide derivative is obtained.Benzoic acid and the urea are mixed and heated for a long time at 220 DEG C, a chemical reaction can be completed only within 20-80 seconds by applying a microwave assistive technology, and the effect higher than the effect achieved by conventional heating is achieved. By applying a solvent-free solid phase method and utilizing an easy-to-obtain reagent, high-yield amide is prepared through a simple and effective method, and the solvent-free solid phase method has the advantages of high reaction speed, low catalyst cost and the like.
Development and Utilization of a Palladium-Catalyzed Dehydration of Primary Amides to Form Nitriles
Al-Huniti, Mohammed H.,Rivera-Chávez, José,Colón, Katsuya L.,Stanley, Jarrod L.,Burdette, Joanna E.,Pearce, Cedric J.,Oberlies, Nicholas H.,Croatt, Mitchell P.
supporting information, p. 6046 - 6050 (2018/09/27)
A palladium(II) catalyst, in the presence of Selectfluor, enables the efficient and chemoselective transformation of primary amides into nitriles. The amides can be attached to aromatic rings, heteroaromatic rings, or aliphatic side chains, and the reactions tolerate steric bulk and electronic modification. Dehydration of a peptaibol containing three glutamine groups afforded structure-activity relationships for each glutamine residue. Thus, this dehydration can act similarly to an alanine scan for glutamines via synthetic mutation.
