Oxidation of aldehydes to carboxylic acids in water catalyzed by cobalt(II) Schiff-base complex anchored to SBA-15/MCM-41

Cobalt(II) Schiff-base complexes were successfully anchored to SBA-15/MCM-41 and used as a catalyst for the oxidation of aldehydes to afford carboxylic acids in water under the action of hydrogen peroxide. Reaction conditions, such as different catalyst type, reaction temperature, reaction time, solvents media, and catalyst amount were studied systematically. High yield (up to 98%) of the process was reached. Such substrate-supported catalyst can be reused up to five times without significant loss of its catalytic activity which is not lower than 85%.     

Formation and Reactivity of Organo‐Functionalized Tin Selenide Clusters

Reactions of R¹SnCl₃ (R¹=CMe₂CH₂C(O)Me) with (SiMe₃)₂Se yield a series of organo‐functionalized tin selenide clusters, [(SnR¹)₂SeCl₄] ( 1 ), [(SnR¹)₂Se₂Cl₂] ( 2 ), [(SnR¹)₃Se₄Cl] ( 3 ), and [(SnR¹)₄Se₆] ( 4 ), depending on the solvent and ratio of the reactants used. NMR experiments clearly suggest a stepwise formation of 1 through 4 by subsequent condensation steps with the concomitant release of Me₃SiCl. Furthermore, addition of hydrazines to the keto‐functionalized clusters leads to the formation of hydrazone derivatives, [(Sn₂(μ‐R³)(μ‐Se)Cl₄] ( 5 , R³=[CMe₂CH₂CMe(NH)]₂), [(SnR²)₃Se₄Cl] ( 6 , R²=CMe₂CH₂C(NNH₂)Me), [(SnR⁴)₃Se₄][SnCl₃] ( 7 , R⁴=CMe₂CH₂C(NNHPh)Me), [(SnR²)₄Se₆] ( 8 ), and [(SnR⁴)₄Se₆] ( 9 ). Upon treatment of 4 with [Cu(PPh₃)₃Cl] and excess (SiMe₃)₂Se, the cluster fragments to form [(R¹Sn)₂Se₂(CuPPh₃)₂Se₂] ( 10 ), the first discrete Sn/Se/Cu cluster compound reported in the literature. The derivatization reactions indicate fundamental differences between organotin sulfide and organotin selenide chemistry.     

Theoretical and experimental studies on a compact stretcher with large spectral bandwidth and high transmission efficiency

To ensure safe and effective amplification for the chirped pulse amplification laser facility, many factors such as pulse spectral width, pulse duration, grating parameters and incidence angle parameter are considered carefully in the design of the pulse stretcher. A compact four pass Offner stretcher design is given out. Experiment results show that the stretcher has broad spectral width, large stretching ratio and high transmission efficiency. By comparison, the calculated result of the dispersion effect on the pulse duration is completely consistent with the experiment result.     

Solventless Formation of G‐Quartet Complexes Based on Alkali and Alkaline Earth Salts on Au(111)

Template cations have been extensively employed in the formation, stabilization and regulation of structural polymorphism of G‐quadruplex structures in vitro. However, the direct addition of salts onto solid surfaces, especially under ultra‐high‐vacuum (UHV) conditions, to explore the feasibility and universality of the formation of G‐quartet complexes in a solventless environment has not been reported. By combining UHV‐STM imaging and DFT calculations, we have shown that three different G‐quartet‐M (M: Na/K/Ca) complexes can be obtained on Au(111) using alkali and alkaline earth salts as reactants. We have also identified the driving forces (intra‐quartet hydrogen bonding and electrostatic ionic bonding) for the formation of these complexes and quantified the interactions involved. Our results demonstrate a novel route to fabricate G‐quartet‐related complexes on solid surfaces, providing an alternative feasible way to bring metal elements to surfaces for constructing metal–organic systems.     

High‐Nuclearity Silver Thiolate Clusters Constructed with Phosphonates

The n‐butylphosphonate ligand has been employed to construct three new silver(I) thiolate compounds. Single‐crystal X‐ray analysis revealed that complexes 1 and 2 are Ag₄₈ and Ag₅₁ coordination chain polymers, while 3 contains a discrete Ag₄₈ cluster, in which three different kinds of silver(I) thiolate cluster shells enclose three different phosphonate‐functionalized silver(I) cluster cores, respectively. The structures of clusters in 1 – 3 feature three three‐shell arrangements, S@Ag₁₂@(nBuPO₃)₉@Ag₃₆S₂₃, S@Ag₁₁@(nBuPO₃)₇(MoO₄)₂ @Ag₄₀S₂₇ and MoO₄@Ag₁₂@(nBuPO₃)₈S₆ @Ag₃₆S₂₄, respectively.     

Separation of isorhamnetin 3‐sulphate and astragalin from Flaveria bidentis (L.) Kuntze using macroporous resin and followed by high‐speed countercurrent chromatography

D4020 resin offered the best dynamic adsorption and desorption capacity for total flavonoids based on the research results from ten kinds of macroporous resin. A column packed with D4020 resin was used to optimize the separation of total flavonoids from Flaveria bidentis (L.) Kuntze extracts. The content of flavonoids in the product was increased from 4.3 to 30.1% with a recovery yield of 90%. After the treatment with gradient elution on D4020 resin, the contents of isorhamnetin 3‐sulfate and astragalin were increased from 0.49 to 8.70% with a recovery yield of 74.1% and 1.16 to 30.8%, with a recovery yield of 92.2%, respectively. Further purification was carried out by one‐run high‐speed countercurrent chromatography yielding 4.5 mg of isorhamnetin 3‐sulfate at a high purity of 96.48% and yielding 24.4 mg of astragalin at a high purity of over 98.46%.     

Development of a magnetic solid‐phase extraction coupled with high‐performance liquid chromatography method for the analysis of polyaromatic hydrocarbons

A novel magnetic solid phase extraction coupled with high‐performance liquid chromatography method was established to analyze polyaromatic hydrocarbons in environmental water samples. The extraction conditions, including the amount of extraction agent, extraction time, pH and the surface structure of the magnetic extraction agent, were optimized. The results showed that the amount of extraction agent and extraction time significantly influenced the extraction performance. The increase in the specific surface area, the enlargement of pore size, and the reduction of particle size could enhance the extraction performance of the magnetic microsphere. The optimized magnetic extraction agent possessed a high surface area of 1311 m²/g, a large pore size of 6–9 nm, and a small particle size of 6–9 μm. The limit of detection for phenanthrene and benzo[g,h,i]perylene in the developed analysis method was 3.2 and 10.5 ng/L, respectively. When applied to river water samples, the spiked recovery of phenanthrene and benzo[g,h,i]perylene ranged from 89.5–98.6% and 82.9–89.1%, respectively. Phenanthrene was detected over a concentration range of 89–117 ng/L in three water samples withdrawn from the midstream of the Huai River, and benzo[g,h,i]perylene was below the detection limit.