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1.
β-Keto esters and acetyl acetone on condensation with glycosylated amino esters in the presence of IR-120 resin resulted in high yields of glycosyl enamino esters or ketones. The latter on cyclisation with NaH in toluene at reflux gave 6-glycosyl-5,6-dihydro-1H-pyridin-4-ones in fair to good yields. 相似文献
2.
Kanchan Upadhyay Anupama Asthana Neetu Tiwari 《Research on Chemical Intermediates》2013,39(6):2629-2640
Two simple and sensitive spectrophotometric methods have been developed for analysis of the antipsychotic drug olanzapine in pharmaceuticals. Method A is based on liberation of iodine by reaction between the drug and potassium iodate, followed by reaction with leuco crystal violet (LCV), the color of oxidized LCV being measured at 598 nm. Method B is based on oxidation of olanzapine with chloramine-T (CAT) in acidic medium, the unconsumed CAT being determined with rhodamine B, measuring the absorbance at 550 nm. Calibration graphs were linear over the ranges of 0.05–2.0 and 0.1–1.6 μg mL?1 olanzapine for method A and B, respectively. The molar absorptivity, Sandell’s sensitivity, detection limit, and quantitation limit were found to be 1.59 × 105, 0.00132, 0.038, and 0.117, respectively, for method A and 0.953 × 105, 0.00221, 0.064, and 0.192, respectively, for method B. The optimum conditions and other analytical parameters were evaluated. The proposed methods have been applied successfully for analysis of olanzapine in pure form and its dosage forms, and no interference was observed from common excipients present in pharmaceutical formulations. 相似文献
3.
Neetu Tiwari Anupama Asthana Kanchan Upadhyay 《Research on Chemical Intermediates》2013,39(8):3867-3875
A simple sensitive extractive spectrophotometric method for determination of trichloroethylene is proposed. Trichloroethylene is treated with pyridine to form glutaconic aldehyde by heterolytic cleavage of the pyridine ring. Glutaconic aldehyde is further coupled with 4-aminoacetanilide to form an orange–red dye which is extractable in 3-methyl-1-butanol. The extracted dye shows absorption maximum at 520 nm. The system obeys Beer’s law in the range of 0.05–0.8 μg mL?1. Important analytical parameters such as time, temperature, reagent concentration, acidity etc. have been optimized for complete colour reaction. Sandell’s sensitivity and molar absorptivity for the system were found to be 0.001 μg cm?2 and 1.2 × 105 L mol?1 cm?1, respectively. The proposed method is satisfactorily applied to micro-level determination of trichloroethylene in various environmental and biological samples. 相似文献
4.
Tetrel bond, a weak noncovalent interaction between the σ-hole of a Group IV element (silicon in our case) and the cloud of an electronegative element (oxygen in our case) is the focus of this work. The percentage strengthening of tetrel bond has been investigated by optimizing 16 binary complexes of halogenated silane and water of general formula SiXnH4−n−H2O and 16 ternary complexes, of general formula NaX−SiXnH4−n−H2O, where X=F, Cl, Br and I and n=1, 2, 3 and 4 at various levels of theory defined within the formalism of density functional theory (DFT). With the addition of NaX, tetrel bond between Si and O in SiXnH4−n−H2O gets strengthened up to 49 %, owing to cooperativity effect exerted by hydrogen bonding between X and H in the ternary complex NaX−SiXnH4−n−H2O. In the series of complexes studied here, overall stabilization due to cooperativity lies between 10 kJ/mol to 170 kJ/mol. This large extent of reinforcement due to cooperativity has never been showcased before. The exceptional stabilization and reinforcement owe its genesis to the transformation of the ternary complex into a cluster orchestrated by the H-bonding in most of the cases and covalent bonding in few of the cases. 相似文献
5.
Neetu Bansal 《Transition Metal Chemistry》2009,34(6):695-702
The kinetics and mechanism of the mercury(II)-catalysed ligand substitution reaction between potassium hexacyanoferrate(II)
and 2-methylpyrazine (2-Mepz), in potassium hydrogen phthalate buffer of pH 3.50 ± 0.02 at 25.0 ± 0.1 °C and constant ionic
strength of 0.1 M, were studied spectrophotometrically by measuring the absorbance of the yellow-coloured product at 447 nm
(λmax). The reaction was studied under pseudo-first-order conditions using excess of 2-Mepz. The reaction was found to obey first-order
dependence in concentration of both [Fe(CN)6]4− and 2-Mepz. At higher concentrations of 2-Mepz, the effect of [2-Mepz] levels off. A complex behaviour is observed on varying
[Hg2+]. The effect of pH on the reaction rate was also analysed. The effects of dielectric constant and water content of the reaction
medium have been interpreted in terms of the formation of a polar activated complex and suggest an Id mechanism. The inhibitory effect of 2,3-dimercaptopropanol on the reaction was also studied and explained in terms of binding
of this species to the catalyst. 相似文献
6.
Amit Kumar Gupta Kumkum Kumari Neetu Singh Dushyant Singh Raghuvanshi Krishna Nand Singh 《Tetrahedron letters》2012,53(6):650-653
An environmentally benign, ionic liquid promoted multicomponent protocol to benzopyrano(2,3-d)pyrimidines and 4H-chromenes has been developed at room temperature. Results of the reaction depend on the nature of the nucleophile used in the reaction. Secondary amines result in the formation of benzopyrano(2,3-d)pyrimidines, whereas thiols give rise to 4H-chromenes under the same set of reaction conditions. 相似文献
7.
ABSTRACT The mixed metal fluorides containing alkali metals have a range of important applications in optical and electronic devices. Raman spectrums of two such fluorides were examined. Raman spectrum of KCuF3 at 300 K exhibited bands at 261, 295, 363, 468, 519, and 549 cm?1, indicating site symmetry (orthorhombic) lower than the tetragonal symmetry as observed from the powder X-ray diffraction pattern. Cubic KNiF3 showed bands at 410, 468, and 657 cm?1. The first two bands were attributed to the second-order phonon scattering, and the band at 657 cm?1 was assigned to two-magnon peak. 相似文献
8.
Sharma A Verma SC Saxena N Chadda N Singh NP Sinha AK 《Journal of separation science》2006,29(5):613-619
Microwave-assisted extraction (MAE), ultrasound-assisted extraction (UAE) and conventional extraction of vanillin and its quantification by HPLC in pods of Vanilla planifolia is described. A range of nonpolar to polar solvents were used for the extraction of vanillin employing MAE, UAE and conventional methods. Various extraction parameters such as nature of the solvent, solvent volume, time of irradiation, microwave and ultrasound energy inputs were optimized. HPLC was performed on RP ODS column (4.6 mm ID x 250 mm, 5 microm, Waters), a photodiode array detector (Waters 2996) using gradient solvent system of ACN and ortho-phosphoric acid in water (0.001:99.999 v/v) at 25 degrees C. Regression equation revealed a linear relationship (r2 > 0.9998) between the mass of vanillin injected and the peak areas. The detection limit (S/N = 3) and limit of quantification (S/N = 10) were 0.65 and 1.2 microg/g, respectively. Recovery was achieved in the range 98.5-99.6% for vanillin. Maximum yield of vanilla extract (29.81, 29.068 and 14.31% by conventional extraction, MAE and UAE, respectively) was found in a mixture of ethanol/water (40:60 v/v). Dehydrated ethanolic extract showed the highest amount of vanillin (1.8, 1.25 and 0.99% by MAE, conventional extraction and UAE, respectively). 相似文献
9.
Prof. Zhenyu Sun Dr. Neetu Talreja Hengcong Tao Prof. John Texter Prof. Martin Muhler Prof. Jennifer Strunk Prof. Jianfeng Chen 《Angewandte Chemie (International ed. in English)》2018,57(26):7610-7627
The transformation of CO2 into fuels and chemicals by photocatalysis is a promising strategy to provide a long‐term solution to mitigating global warming and energy‐supply problems. Achievements in photocatalysis during the last decade have sparked increased interest in using sunlight to reduce CO2. Traditional semiconductors used in photocatalysis (e.g. TiO2) are not suitable for use in natural sunlight and their performance is not sufficient even under UV irradiation. Some two‐dimensional (2D) materials have recently been designed for the catalytic reduction of CO2. These materials still require significant modification, which is a challenge when designing a photocatalytic process. An overarching aim of this Review is to summarize the literature on the photocatalytic conversion of CO2 by various 2D materials in the liquid phase, with special attention given to the development of novel 2D photocatalyst materials to provide a basis for improved materials. 相似文献
10.
Nanoparticles possessing multiple functionalities provide synthetic handles for varied surface chemistries, making them useful for a range of applications such as biotargeting and drug delivery. However, the combination of interfering functionalities on the same particle is often challenging. We have employed a synthetic scheme involving chemical protection/deprotection to combine interfering functional groups on the same hydrogel nanoparticle. The synthesis of amine-containing poly(N-isopropylacrylamide) nanogels was carried out via free radical precipitation polymerization by incorporating a Fmoc-protected amine poly(ethylene glycol) (PEG) macromonomer. The Fmoc group was then removed to obtain free amines, which were shown to be available for conjugation. We further explored pNIPAm-co-acrylic acid nanogels with a protected amine-PEG, yielding zwitterionic particles. With careful attention to the order of the chemoligation and deprotection steps, these interfering functional groups can be forced to behave in a pseudo-orthogonal fashion, allowing for multiple chemoligation steps that employ both the amine and carboxylic acid groups. 相似文献