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An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

Section 1.1 General InformationChalcones 1 and enamine 2a were prepared according to reported procedures. 1,2All other chemical reagents were obtained from commercial suppliers and used without further purification.The mixer mill MM 400 (Retsch GmbH, Germany) was used for all ball-milling reactions, and the reaction vessels are titanium-alloyed jars lined with PTFE (neat volume: 4 mL) or stainless jars (neat volume: 25 mL).The milling balls are titanium-alloyed of 6.0 mm in diameter or stainless of 8.0 mm in diameter.Analytical thin-layer chromatography was performed on glass plates pre-coated with silica gel impregnated with a fluorescent indicator (254 nm), and the plates were visualized by exposure to ultraviolet light.Column chromatography was performed on silica gel using EtOAc/petroleum ether as the eluent.Melting points were determined on a XT-4 binocular microscope (Beijing Tech Instrument Co., China) and are uncorrected. 1H NMR spectra were recorded on a Bruker AV300, AV400 or AV500 NMR instrument.Chemical shifts are reported in parts per million with the solvent resonance as the internal standard (CDCl 3 , δ 7.26). 13C NMR spectra were recorded on an NMR instrument operated at 125 MHz or 100 MHz with complete proton decoupling.Chemical shifts are reported in parts per million with the solvent resonance as the internal standard (CDCl 3 , δ 77.16).HR-MS were recorded on a Bruker MicroTOF-QII mass instrument (ESI). General Procedure for the Synthesis of Product 5 (5a as an Example)Aniline (3a, 0.55 mmol), ethyl acetoacetate (4a, 0.55 mmol), AlCl 3 (0.125 mmol), together with two titanium-alloyed balls of 6.0 mm in diameter, were introduced into a titanium-alloyed jar lined with PTFE (4 mL).The same mixture was also introduced into a second parallel jar.The two reaction vessels were sealed with screw caps, fixed on the vibration arms of a ball-milling apparatus (mixer mill MM400, Retsch GmbH, Haan, Germany) and were vibrated vigorously at a rate of 1800 rounds per minute (30 Hz) at room temperature for 30 minutes.After the vessels were opened, chalcone (1a, 0.5 mmol) and AlCl 3 (0.25 mmol) were added into the two parallel jars, respectively.The vessels were sealed again and continued to vibrate for 60 minutes (30 Hz).The resulted mixtures were combined and directly loaded on silica gel chromatography column for purification with EtOAc/petroleum ether as the eluent, affording the desired product 5a as white solid. General Procedure for the Synthesis of Product 6 (6a as an Example)

Abstract Three new C 15 acetogenins (I)—(III) are isolated from the ether extract of the red alga Laurencia obtusa along with one known compound.

RuO 2 nanoparticles decorated TiO 2 nanobelt on titanium plate is active for electrocatalytic hydrogen evolution, requiring overpotentials of 130, 143, and 380 mV to drive 100 mA cm −2 in 0.5 M H 2 SO 4 , 1.0 M KOH, and 1.0 M PBS solution, respectively.

Abstract The synthesized MgTi 2 O 4 ⋅TiO 2 ⋅Zn 2 TiO 4 nanomaterial was characterized by XRD (X‐Ray diffraction), SEM (Scanning electron microscopy), EDS (Energy dispersive x‐ray spectroscopy), FTIR (Fourier transform infrared spectroscopy) and PL (Photoluminescence) study. Particles size of MgTi 2 O 4 ⋅TiO 2 ⋅Zn 2 TiO 4 nanomaterial was found to be 37.3 nm. PL and PLE (Photoluminescence excitation) spectra are showed several peaks including one red PL at 723 nm, when excited at 320 nm. Nanomaterial was subject to electrochemical sensor study. Thin layer of synthesized MgTi 2 O 4 ⋅TiO 2 ⋅Zn 2 TiO 4 nanomaterials was fabricated onto the glassy carbon electrode (GCE) with conducting binder to result the working electrode of 4‐nitrophenylhydrazine (4‐NPHyd) sensor, which was applied successively to selectively detect the 4‐NPHyd in aqueous phase. The 4‐NPHyd chemical sensor exhibited high sensitivity with lower detection limit, long‐term stability in chemical environment and improved electrochemical responses during sensing performance. The linearity of calibration plot is obtained over the large linear dynamic range (LDR) from 0.1 nM to 0.1 mM of 4‐NPHyd. The sensitivity calculated from the slop of calibration plot (ratio of current to concentration of 4‐NPHyd) is 42.7215 μAmM −1 cm −2 with detection limit (DL) of 0.02±0.001 nM at signal to noise ratio of 3(S/N). Therefore, the chemical sensor based on MgTi 2 O 4 ⋅TiO 2 ⋅Zn 2 TiO 4 nanomaterials may be a promising highly sensitive sensor in electrochemical method for the effective detection of hazardous and carcinogenic chemicals in medical as well as biological sectors.

Two simple and sensitive kinetic methods for the determination of ampicillin (AMP) are described. The first method is based on kinetic investigation of the oxidation reaction of the drug with alkaline potassium permanganate at room temperature for a fixed time of 25 min. The absorbance of the colored manganate ions is measured at 610 nm. The second method is based on the reaction of AMP with 1-chloro-2,4-dinitrobenzene (CDNB) in the presence of 0.1 mol L−1 sodium bicarbonate. Spectrophotometric measurement was achieved by recording the absorbance at 490 nm for a fixed time of 60 min. All variables affecting the development of the color were investigated and the conditions were optimized. Plots of absorbance against concentration in both procedures were rectilinear over the ranges 5–30 and 50–260 μg mL−1, with mean recoveries 99.80 and 99.91, respectively. The proposed methods were successfully applied for the determination of AMP in bulk powder and in capsule dosage form. The determination of AMP by the fixed concentration method is feasible with the calibration equations obtained, but the fixed time method proves to be more applicable.

In recent years, a new class of highly crystalline advanced permeable materials covalent-organic frameworks (COFs) have garnered a great deal of attention thanks to their remarkable properties, such as their large surface area, highly ordered pores and channels, and controllable crystalline structures. The lower physical stability and electrical conductivity, however, prevent them from being widely used in applications like photocatalytic activities and innovative energy storage and conversion devices. For this reason, many studies have focused on finding ways to improve upon these interesting materials while also minimizing their drawbacks. This review article begins with a brief introduction to the history and major milestones of COFs development before moving on to a comprehensive exploration of the various synthesis methods and recent successes and signposts of their potential applications in carbon dioxide (CO₂ ) sequestration, supercapacitors (SCs), lithium-ion batteries (LIBs), and hydrogen production (H₂ -energy). In conclusion, the difficulties and potential of future developing with highly efficient COFs ideas for photocatalytic as well as electrochemical energy storage applications are highlighted.