We describe an efficient continuous flow synthesis of ketones from CO2 and organolithium or Grignard reagents that exhibits significant advantages over conventional batch conditions in suppressing undesired symmetric ketone and tertiary alcohol byproducts. We observed an unprecedented solvent-dependence of the organolithium reactivity, the key factor in governing selectivity during the flow process. A facile, telescoped three-step-one-flow process for the preparation of ketones in a modular fashion through the in-line generation of organometallic reagents is also established.
A novel Salen-type bisoxime ligand, 6,6¢-dimethoxy-2,2¢-[(1,4-butylene)dioxybis(nitrilomethylidyne)]diphenol (H 2 L) and its tetranuclear Cu(II) complex, [Cu 4 L 2 (pic) 4 (H 2 O) 2 ]AE2H 2 O, have been synthesized and characterized by elemental analyses, IR, TG-DTA and 1 H-NMR etc. The X-ray crystal structure of the complex reveals that formation of a tetranuclear structure, which consists of four copper(II) atoms, two pentadentate L 2) units, four picratols, two coordinated water molecules and two crystallizing water molecules. Around four copper ions are all octahedral geometries. It was demonstrated that the picratols in the tetranuclear copper(II) complex show a novel tridentate coordination mode.
By coupling the self-assembly of polystyrene-block-poly(ethylene oxide)-containing titanium-tetraisopropoxide and tungsten hexaphenoxide (the precursors of TiO 2 and WO 3 , respectively) with electrospinning technique, the hierarchically porous TiO 2 /WO 3 composite nanofibers with inner-bicontinuous and outer-shell structures have been synthesized. Scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy were employed to characterize the structure of the fibers. In these nanofibers, the TiO 2 acts as the frames, and WO 3 fills the gaps. The UV−vis spectroscopy suggests that the spectral response range has been successfully extended into the visible regime. Furthermore, the resulting fabrics show enhanced performance in the photocatalytic degradation of acetaldehyde relative to neat TiO 2 and neat WO 3 . Our results indicate that electrospinning the blend solution of block copolymer and two kinds of precursor of inorganic material is an effective strategy to fabricate composite nanofibers that can improve the photocatalytic activity of TiO 2 , especially for visible light.
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