An efficient and convenient methodology has been developed for the conversion of 2-hydroxy phenyl ketoxime to 1,2-benzisoxazole 2-oxide with sodium perborate (SPB) in glacial acetic acid under mild reaction conditions. Interestingly when the reaction was carried out under reflux condition deoximation was observed in quantitative yield. 相似文献
A rapid and sensitive gas chromatographic method using flame ionization detection (GC–FID) has been developed and validated for five process related non-chromophoric impurities viz, 2-(2-chloroethoxy)ethanol (2-CEE), piperazine, 2-(piperazin-1-yl)ethanol (HEP), 2-[2-(piperazin-1-yl)ethoxy]ethanol (HEEP), 2,2-[piperazine-1,4-diylbis(ethane-2,1-diyloxy)]diethanol (DEEP) observed during the process development of quetiapine hemifumarate, an antipsychotic drug is presented. All five non-chromophoric impurities ranging from 0.05 to 0.1% were detected using DB-5 (30 m × 0.53 mm, 5 μm) column with a good peak separation. The method was fully validated according to the ICH Q2 (R1) guidelines. The investigated validation protocols showed that the method has acceptable specificity, accuracy, linearity, precision, robustness and high sensitivity with detection limits and quantitation limits ranging from 0.001 to 0.01% and 0.004 to 0.03%, respectively. These non-chromophoric impurities generated during the process were identified by GC–MS and are characterized by MS, 1H NMR and FT-IR spectroscopy.
Spinal ferrites having the general formula Co1 − xZnxFe2 − xAlxO4 (x = 0.0, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6) were prepared using the wet chemical co-operation technique. The samples were annealed
at 800°C for 12 h and were studied by means of X-ray diffraction, magnetization and low field AC susceptibility measurements.
The X-ray analysis showed that all the samples had single-phase cubic spinel structure. The variation of lattice constant
with Zn and Al concentration deviates from Vegard’s law. The saturation magnetization σs and magneton number nB measured at 300 K using high field hysteresis loop technique decreases with increasing x, suggesting decrease in ferrimagnetic behaviour. Curie temperature TC deduced from AC susceptibility data decreases with x, suggesting a decrease in ferrimagnetic behaviour.
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An efficient synthesis of substituted 1-pyridylimidazo-[1,5-a]-pyridines has been accomplished using scandium(III) triflate as catalyst under mild conditions in excellent yields. 相似文献
ABSTRACT Thermally grown SiO2 thin films on a silicon substrate implanted with 100?keV silicon negative ions with fluences varying from 1?×?1015 to 2?×?1017 ions cm?2 have been investigated using Electron spin resonance, Fourier transforms infrared and Photoluminescence techniques. ESR studies revealed the presence of non-bridging oxygen hole centers, E′-centers and Pb-centers at g-values 2.0087, 2.0052 and 2.0010, respectively. These vacancy defects were found to increase with respect to ion fluence. FTIR spectra showed rocking vibration mode, stretching mode, bending vibration mode, and asymmetrical stretching absorption bands at 460, 614, 800 and 1080?cm?1, respectively. The concentrations of Si–O and Si–Si bonds estimated from the absorption spectra were found to vary between 11.95?×?1021 cm?3 and 5.20?×?1021 cm?3 and between 5.90?×?1021 cm?3 and 3.90?×?1021 cm?3, respectively with an increase in the ion fluence. PL studies revealed the presence of vacancies related to non-bridging oxygen hole centers, which caused the light emission at a wavelength of 720?nm. 相似文献
The emergence and development of aggregation induced emission (AIE) have attracted worldwide attention due to its unique photophysical phenomenon and for removing the obstacle of aggregation-caused quenching (ACQ) which is the most detrimental process thereby making AIE an important and promising aspect in various fields of fluorescent material, sensing, bioimaging, optoelectronics, drug delivery system, and theranostics. In this review, we have discussed insights and explored recent advances that are being made in AIE active materials and their application in sensing, biological cell imaging, and drug delivery systems, and, furthermore, we explored AIE active fluorescent material as a building block in supramolecular chemistry. Herein, we focus on various AIE active molecules such as tetraphenylethylene, AIE-active polymer, quantum dots, AIE active metal-organic framework and triphenylamine, not only in terms of their synthetic routes but also we outline their applications. Finally, we summarize our view of the construction and application of AIE-active molecules, which thus inspiring young researchers to explore new ideas, innovations, and develop the field of supramolecular chemistry in years to come. 相似文献
The use of ordinary Portland cement (OPC) in the construction industry is inevitable. The huge production of OPC and its use in infrastructural development pose an environmental impact. Greenhouse gas emitted increases the global temperature and it is an alarming sign to everybody on the planet. Concrete is the most consuming material which is produced by using OPC and it is proven that OPC contributes a lot to CO2 emission. Hence in this study attempt is made to produce concrete by using environment-friendly material like fly ash along with alkaline activators, which is termed Geo polymer concrete. The by-product fly ash is widely available worldwide. It is a by-product of thermal power plants. The use of fly ash in concrete produces less expensive and more cost-effective concrete than concrete made up using OPC. Due to its high silicate and alumina content, fly ash reacts with an alkaline solution to create an aluminosilicate gel that binds the aggregate and results in high-quality concrete. Fly ash is finer than cement, it occupies the pores of cement after hydration. This would result in denser concrete which gives higher strength. In comparison to ordinary concrete, fly ash-based geopolymer concrete offers better resistance to aggressive environments and high temperatures. In the present study, an alkaline activator of molarity 8 is used to prepare geopolymer concrete. The test specimens are cast and cured for 28 days. Test results indicate that an alkaline liquid fly-ash ratio (0.4) produces higher mechanical properties. Hence, geopolymer concrete produced in this study is found to be cost-effective and environment friendly. 相似文献
New silicon containing azopolyamides have been prepared from 4,4′-diaminoazobenzene and four structurally related organosilicon acid dichlorides. Polymerization was carried out by the technique of low temperature interfacial polycondensation using methylene chloride-water system. The polymers were yellow to brown in colour. They were characterized by visible and i.r. spectroscopy, X-ray diffraction, solubility and by solution viscosity. Thermal behaviour of these polyamides was studied by dynamic thermogravimetry. 相似文献