626-17-5Relevant articles and documents
Catalytic activity of vanadium-substituted molybdophosphoric acid supported on titania for the vapor-phase synthesis of isophthalonitrile
Senapati,Dutta,Rana, Surjyakanta,Parida,Sahu,Sarkar
, p. 1429 - 1435 (2017)
Different wt% of vanadium-substituted molybdophosphoric acid H4PMo11VO40 loaded on titania (TiO2) are prepared by wet impregnation method. The catalytic activity of PMoV-supported titania catalyst for the vapor-phase ammoxidation of m-xylene at different temperatures is reported here. The synthesized catalysts were characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction, N2 adsorption–desorption, thermogravimetric/differential thermal analysis, temperature programmed desorption (TPD), temperature programmed reduction (TPR) scanning electron microscopy, energy-dispersive X-ray spectroscopy (EDX), and transmission electron microscopy?(TEM). FTIR studies confirmed that the Keggin structure of PMoV does not change even up to 460°C when loaded on TiO2 surface. Among all the PMoV-supported TiO2 catalysts, 1.7% PMoV/TiO2 showed excellent activity for vapor-phase ammoxidation of m-xylene with 85.4% yield of isophthalonitrile.
Visible-Light-Promoted Metal-Free Synthesis of (Hetero)Aromatic Nitriles from C(sp3)?H Bonds**
Murugesan, Kathiravan,Donabauer, Karsten,K?nig, Burkhard
supporting information, p. 2439 - 2445 (2020/12/07)
The metal-free activation of C(sp3)?H bonds to value-added products is of paramount importance in organic synthesis. We report the use of the commercially available organic dye 2,4,6-triphenylpyrylium tetrafluoroborate (TPP) for the conversion of methylarenes to the corresponding aryl nitriles via a photocatalytic process. Applying this methodology, a variety of cyanobenzenes have been synthesized in good to excellent yield under metal- and cyanide-free conditions. We demonstrate the scope of the method with over 50 examples including late-stage functionalization of drug molecules (celecoxib) and complex structures such as l-menthol, amino acids, and cholesterol derivatives. Furthermore, the presented synthetic protocol is applicable for gram-scale reactions. In addition to methylarenes, selected examples for the cyanation of aldehydes, alcohols and oximes are demonstrated as well. Detailed mechanistic investigations have been carried out using time-resolved luminescence quenching studies, control experiments, and NMR spectroscopy as well as kinetic studies, all supporting the proposed catalytic cycle.
Recyclable and Reusable Pd(OAc)2/XPhos–SO3Na/PEG-400/H2O System for Cyanation of Aryl Chlorides with Potassium Ferrocyanide
Cai, Mingzhong,Huang, Bin,Liu, Rong,Xu, Caifeng
, (2021/12/03)
Pd(OAc)2/XPhos–SO3Na in a mixture of poly(ethylene glycol) (PEG-400) and water is shown to be a highly efficient catalyst for the cyanation of aryl chlorides with potassium ferrocyanide. The reaction proceeded smoothly at 100 or 120?oC with K2CO3 or KOAc as base, delivering a variety of aromatic nitriles in good to excellent yields. The isolation of the crude products is facilely performed by extraction with cyclohexane and more importantly, both expensive Pd(OAc)2 and XPhos–SO3Na in PEG-400/H2O system could be easily recycled and reused at least six times without any apparent loss of catalytic efficiency. Graphical Abstract: Palladium-catalyzed cyanation of aryl chlorides with potassium ferrocyanide leading to aryl nitriles by using Pd(OAc)2/XPhos–SO3Na/PEG-400/H2O as a highly efficient and recyclable catalytic system is described.[Figure not available: see fulltext.]
