Palladium nanoparticle-incorporated metal-organic framework MIL-101 (Pd/MIL-101) was successfully synthesized and characterized using X-ray diffraction, nitrogen physisorption, X-ray photoelectron, UV-visible and infrared spectroscopies, and transmission electron microscopy. The characterization techniques confirmed high porosity and high surface area of MIL-101 and high stability of nano-size palladium particles. Pd/MIL-101 nanocomposite was investigated for the Sonogashira cross-coupling reaction of aryl and heteroaryl bromides with various alkynes under copper-free conditions. The reusability of the catalyst was tested for up to four cycles without any significant loss in catalytic activity.
Three-dimensional mesoporous silica
with a highly dispersed palladium
nanoparticles composite (PS-3) catalyst has been prepared and characterized
by X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform
infrared spectroscopy, nitrogen sorption, and high resolution transmission
electron microscopy. The PS-3 catalyst utilized for the first time
as an efficient and reusable catalyst in the ortho-arylation of benzamides by aryl iodides has been demonstrated with
the simplest amide CONH2 as a directing group. It can be
successfully applied to various benzamides and aryl iodides with both
electron donating and withdrawing groups. The catalyst can be simply
recovered and reused several times without significant loss in catalytic
activity.
A C–O bond‐formation reaction that proceeds through C–H functionalization of N,N‐dialkylanilines at the ortho‐position is presented. The iron‐catalyzed selective ortho‐benzoyloxylation follows a polar Friedel–Crafts‐like mechanism and is sensitive to the nucleophilicity of the anilines. The benzoyloxylation of a variety of N,N‐disubstituted anilines and N‐phenyl heterocycles is carried out under extremely mild conditions. Furthermore, the methodology has been successfully employed for the generation of 1,4‐benzoxazepines and o‐aminophenols.
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