Utility of N‐[4‐(N‐Substituted Sulfamoyl)Phenyl] Cyanothioformamides in the Synthesis of Heterocyclic Compounds

The novel cyanothioformamides 2a‐d were prepared by treatment of isothiocyanatosulfonamides 1a‐d with potassium cyanide at room temperature. Cyclocondensation of compounds 2b,c with phenyl isocyanate as electrophile furnished the corresponding imidazolidines 3a,b . The reactivity of compound 3a towards some nitrogen nucleophiles was investigated. Thus, the thiosemicarbazone 4 and imidazo[4,5‐b]quinoxaline 6 were synthesized by condensation of compound 3a with thiosemicarbazide and o‐phenylenediamine, respectively. Treatment of 3a with hydrochloric acid afforded compound 7 . Our investigation was extended to include the reactivity of cyanothioformamide 2 towards o‐aminophenol, anthranilic acid, and o‐phenylenediamine and yielded the corresponding heterocycles 9 , 11 and 13 derivatives, respectively. Structures of the synthesized compounds were established by their elemental analysis and spectral data.     

De novo enantioselective syntheses of galacto-sugars and deoxy sugars via the iterative dihydroxylation of dienoate

An efficient route to various sugar lactones has been developed. Key to the overall transformation is the sequential osmium-catalyzed dihydroxylation of 2,4-dienoates. The simplest (one-step/racemic) example of this reaction occurs when the dihydroxylation is performed with aqueous NMO in MeOH. When the first dihydroxylation is performed using the AD-mix procedure, an enantioselective variant results. When a matched AD-mix procedure is used for the second dihydroxylation, an exceedingly diastereo- and enantioselective synthesis of galacto-1,4-lactone results. [Reaction: see text]     

Quantum chemical studies on structures and spectra of 2,5-distyrylpyrazine (DSP) laser dye

Semiempirical (MNDO and PM3) molecular orbital calculations have been undertaken to study the structures of the ground and excited states of 2,5-distrylpyrazine dye to assess its activity as a laser dye. In the ground and first excited singlet states, the trans-trans structure of C_2h symmetry is the most stable structure in the gas phase and in DMSO, which agrees with the experimental findings. Upon excitation, the flexibility of the molecule decreases, leading to a subsequent decrease in the radiationless deactivation pathway and this increases the fluorescence efficiency of DSP. The absorption, excitation, and emission spectra have been calculated at the MNDO level using the PM3 optimized geometries in DMSO. At this level the agreement between theory and experiment is quite good. An estimated absorption band at 377 nm (expt 380 nm) is assigned to the S₀→S₁ transition. The excited state absorption band at 457 nm (expt 460 nm) is assigned to the S₁→S₁₂ transition. The emission band at 458 nm (expt 460 nm) is assigned to the S′₁→S′₀ transition. The overlap between the emission and the excited-state absorption spectra is presumably the main reason behind the reduced laser activity of the investigated dye. © 1998 John Wiley & Sons, Inc. J Comput Chem 19: 585–592, 1998     

Inhibition of Pb-Leaching from Lead Crystal Glass by Coating with Films Prepared by the Sol-Gel Method

The chemical durability of lead glass tumblers (24% PbO) in a 4% (v/v) acetic acid solution before and after coating with sol-gel derived SiO2 films was assessed to determine the extent of reduction in Pb-leaching that can be achieved. It was found that by coating the internal surface of the glass tumblers with 1 ml of 10% TEOS solutions at 100°C and densifying the coating formed at 500°C for 1 h, it was possible to reduce Pb-leaching to about one quarter of that of the uncoated glass.     

A Microwave Assisted Diazo Coupling Reaction: The Synthesis of Alkylazines and Thienopyridazines

Heating diazoaminobenzene with active methylene compounds 1–3 in microwave oven in acetic acid, in the presence of hydrochloric acid, afforded the corresponding arylhydrazones 5–7. These reaction products were condensed with ethyl cyanoacetate in a domestic microwave oven after 1–2 minutes heating to yield the pyridazinones 8–12. Compounds 8c and 12 reacted with sulfur in basic DMF solution, in microwave oven using MORE technology to yield the thienopyridazinone 14 and 16 respectively. While 17 was produced when 8b was treated like wise with sulfur and DMF in the presence of piperidine. Compounds 16 coupled with aromatic diazonium salts to yield arylazo derivatives 21a–c.     

Synthesis and Characterization of Carbohydrate-Copolyhydrazides Containing Ether Bonds in the Monomer Unit

Abstract

A series of carbohydrate-containing copolyhyrazides having ether bonds were prepared by low temperature solution polycondensation. 2,3,4,5-tetra-O-acetyl galactaroyl dichloride was polycondensed with hydroquinone-1,4-diacetic acid dihydrazide (1), 2-bromo-,2-chloro, 2-nirohydroquinone-1,4-diacetic acid dihydrazide (2, 3 and 4, respectively) and isophthaloyl dihydrazide (5) in dimethylformamide and produced copolyhydrazides (6-10), respectively. Copoly {1-[2-(2,3,4,5-tetra-O-acetyl-galacto-tetritoldi-1,4-yl)-5-(1,3,4-oxadiazol-di-2,5-yl]-3-[2-(1,3,4-oxadiazole-di-2,5-yl)-benzene]}(11)wassynthesizedbydehydrative cyclisation of the polymer(10) using thionyl chloride. Also, polymer (10), under de-O-acetylation in methanolic ammonia, gave the de-O-acetylated polymer (12). All the present new polymers were characterized by elemental analysis and i.r. and ¹H-NMR spectroscopy. Their solubility, viscosity and physical properties are studied.     

Three Validated Methods for Simultaneous Determination of Ofloxacin and Dexamethasone in Binary Mixture

JPC – Journal of Planar Chromatography – Modern TLC - Three selective, precise, and accurate methods were developed and validated for the simultaneous determination of ofloxacin and...     

Chemical studies on uranium extraction from concentrated phosphoric acid by using PC88A and DBBP mixture

The activity concentration of beryllium-7 (⁷Be), a naturally occurring cosmogenic radionuclide produced in the upper atmosphere, was measured in plants on the Loess plateau of China during the growing season of 2005. The ⁷Be mass activity concentration on July 27 ranged from 34.8 to 147.1 Bq kg⁻¹ in herbaceous plants, from 47.6 to 116.1 Bq kg⁻¹ in subshrubs, and from 15.7 to 56.8 Bq kg⁻¹ in crop plants. The ⁷Be mass and areal activity concentrations of a mixture of herbaceous plants increased from 66.8 to 288.7 Bq kg⁻¹ and from 0.7 to 46.5 Bq m⁻², respectively, during the growing season. On an areal basis, the fraction of ⁷Be in plants in the soil–plant system increased from 0.4 to 8.4% during the growing season. Positive linear correlations were found between the increases of ⁷Be mass and areal activity concentrations in the inter-sampling intervals and the amount of precipitation.