A facile synthesis of novel spiroindane-1,3-diones has been achieved via 1,3-dipolar cycloaddition of an azomethine ylide, generated in situ from ninhydrin and 1,2,3,4-tetrahydroisoquinoline, with the conjugated double bond of chalcone derivatives. The regiochemistry and structures of the cycloadducts were determined with spectroscopic data and by X-ray crystal structure analysis. 相似文献
Rapid, inexpensive, and efficient sample-preparation by dispersive liquid–liquid microextraction (DLLME) then gas chromatography with flame ionization detection (GC–FID) have been used for extraction and analysis of BTEX compounds (benzene, toluene, ethylbenzene, and xylenes) in water samples. In this extraction method, a mixture of 25.0 μL carbon disulfide (extraction solvent) and 1.00 mL acetonitrile (disperser solvent) is rapidly injected, by means of a syringe, into a 5.00-mL water sample in a conical test tube. A cloudy solution is formed by dispersion of fine droplets of carbon disulfide in the sample solution. During subsequent centrifugation (5,000 rpm for 2.0 min) the fine droplets of carbon disulfide settle at the bottom of the tube. The effect of several conditions (type and volume of disperser solvent, type of extraction solvent, extraction time, etc.) on the performance of the sample-preparation step was carefully evaluated. Under the optimum conditions the enrichment factors and extraction recoveries were high, and ranged from 122–311 to 24.5–66.7%, respectively. A good linear range (0.2–100 μg L−1, i.e., three orders of magnitude; r2 = 0.9991–0.9999) and good limits of detection (0.1–0.2 μg L−1) were obtained for most of the analytes. Relative standard deviations (RSD, %) for analysis of 5.0 μg L−1 BTEX compounds in water were in the range 0.9–6.4% (n = 5). Relative recovery from well and wastewater at spiked levels of 5.0 μg L−1 was 89–101% and 76–98%, respectively. Finally, the method was successfully used for preconcentration and analysis of BTEX compounds in different real water samples.
<正>A new practical method for the synthesis of unsymmetrical ureas was achieved by reaction of phenylurea with primary and secondary amines under neutral and mild condition in very good yields.The reaction took place in refluxing dioxane and does not require any catalyst or additives. 相似文献
A mild and efficient method for the copper-catalyzed arylation of phenylurea is described. The coupling reaction of phenylurea with different functionalized aryl iodides in the presence of air stable CuI, N,N′-dibenzylethylenediamine as a ligand, and KF/Al2O3 as a base gives symmetrical and unsymmetrical diarylureas in relatively high yields. 相似文献
Research on Chemical Intermediates - MCM-41-SO3H, ordered mesoporous silica material MCM-41 with covalently anchored sulfonic acid groups, was used as a solid acid catalyst for the convenient,... 相似文献
Some new amidated fentanyl (=N‐[1‐(2‐phenylethyl)piperidin‐4‐yl]‐N‐phenylpropanamide) analogs with a 4‐(N‐phenylamido)piperidine scaffold and additional amide bonds have been designed and synthesized through Ugi four‐component reaction (Ugi‐4CR). Good‐to‐high yields, diversity‐oriented synthesis, and possible applications in drug discovery are advantages of this approach. 相似文献
The application of the recently introduced dispersive liquid–liquid microextraction (DLLME) for the separation and determination of an inorganic selenite [Se(IV)] derivative by means of a gas chromatography–electron-capture detection system has been studied. The selenium derivative was extracted with the DLLME technique using a mixture of ethanol (disperser solvent) and chlorobenzene (extraction solvent). The influences of the various analytical parameters on the derivatization reaction and microextraction procedure have been evaluated and optimized. Under the optimum conditions, an enrichment factor of 122 was obtained for only 5.00 mL of the water sample. The calibration graph was linear in the range of 0.015–10 μg L?1 with a detection limit of 0.005 μg L?1. The relative standard deviation for ten replicate measurements of 2 μg L?1 of selenium was 4.1%. The method was applied to the determination of selenium in environmental surface water samples with satisfactory recovery. 相似文献
Journal of Thermal Analysis and Calorimetry - This study was conducted with the aim of investigating the Newtonian nanofluid flow in a catheterized tapered artery through using a completely... 相似文献