Three-component coupling of alkynes, Baylis-Hillman adducts and sodium azide: a new synthesis of substituted triazoles

A three-component coupling was used to prepare a series of 1,4-disubstituted-1,2,3-triazoles from the corresponding acetylated Baylis-Hillman adducts, sodium azide and terminal alkynes. This one-pot reaction further increases the efficacy of ‘Click’ synthesis and diversifies the preparation of multi-functional 1,4-disubstituted-1,2,3-triazoles.     

Perturbed sites and host—guest—host exciton cascade in the biphenyl isotopic mixed crystal phosphorescence

An interesting energy cascade is observed in the phosphorescence spectra of 1% biphenyl-h₁₀ in biphenyl-d₁₀ (2–15 K); strongly perturbed host sites, with energy levels below that of the protonated guest, quench the guest sites at higher temperatures (11–15 K). The identification of the perturbed sites is based on vibrational characteristics (both intensity and frequency), obtained with the help of phosphorescence spectra of biphenyl-h₁₀ and biphenyl-d₁₀ in an argon matrix, indicating an isotope dependent vibronic structure. A partial vibrational analysis is presented, resulting in confirmation of the first triplet state of biphenyl as orbitally ungerade. The dynamics of the triplet excitation are discussed, including several possible mechanisms explaining the non-Boltzmann nature of the low-temperature steady state.     

Extractive spectrophotometric determination of some fluoroquinolone derivatives in pure and dosage forms

Two simple and sensitive extractive spectrophotometric methods for the determination of some fluoroquinolone derivatives (norfloxacin, NRF; ciprofloxacin, CPF; ofloxacin, OFL; and enrofloxacin, ERF) with Supracene Violet 3B (SV 3B, method A) and tropaeolin 000 (TP 000, method B) are described. The methods are based on the formation of ion-association complexes of fluoroquinolones with these dyes, which are extracted into chloroform and have absorption maxima at 575 nm (SV 3B) and 485 nm (TP 000). The methods obey Beer's law and the precision and accuracy of the methods were checked by UV reference methods. The detection limits were 5.0 mug/ml for NRF and 2.5 mug/ml for CPF in method A and 2.5 mug/ml for OFL and ERF in methods A and B.     

Survival probability in one dimension for theA+B→B reaction with hard-core repulsion

We study the effect of hard-core repulsion (known as the bus effect) betweenB particles on the reaction-diffusion systemA+BB in the continuous-time random walk model in one dimension with theA particles stationary. We show rigorously that the survival probability of theA particles is asymptotically bounded asC ₁lim _t{[–logS(t)]/t ^0.5}C ₂, whereC ₁ andC ₂ are constants. We also do simulations to confirm our results.     

Evaluation of the quality of colour changes of complexometric indicators in the titration of copper (II) with EDTA by tristimulus colorimetry

The quality of colour changes of the indicators hematoxylin, 4(2-pyridylazo)resorcinol (PAR), xylenol orange, pyrocatechol violet, chromazurolS and eriochrome cyanineR in the complexometric titration of copper(II) with ethylenediaminetetraacetic acid (EDTA) were studied with the help of tristimulus colorimetry, utilising a comparative study of the parameters SCD (specific colour discrimination), CIE La^*b^* 1976 and LABHNU 1977. Hematoxylin was found to be the best indicator among those studied. A screened indicator, viz. PAR + malachite green (52), was developed to enhance the quality of colour transition at the end-point and the accuracy of the titrimetric determination.     

Structures of two ketals derived from a pentacyclic cage diketone

The structure of a compound derived from a symmetrical cage diketone in which one of the ketone C=O groups has been converted into a ketal is reported. An investigation into reasons for the selective functionalization resulted in the isolation of acis, cisoid, cis linear triquinane derivative in which both ketones are converted to ketals that share a transannular oxygen atom. Crystal data:2, monoclinic,P2₁/c,a=7.6298(9),b=7.673(3),c=22.125(3)Å,=97.59(1)°,V=1283.9(5)ų, andR=0.048 (1001 reflections);4, triclinic,P¯1,a=7.3864(9),b=9.6362(9),c=10.3889(9)Å,=75.749(6),=76.300(8), =83.100(8)°,V=694.8(4)ų, andR=0.088 (1284 reflections).     

Triplet excition emissions of octafluoronaphthalene crystalline complexes with naphthalene and durene

The phosphorescence spectra of naphthalene-octafluoronaphthalene and durene-octafluoronaphthalene at 4.2 K reveal a localized exciton emission from octafluoronaphthalene, a weak intercomponent triplet-states quasi-resonance and a weak exciton-phonon coupling.     

A statistical model for the optimization of dsc performance in the evaluation of drugs for preformulation studies

Differential scanning calorimetry (DSC) is a thermal analytical tool for preformulation studies. Extrapolated melting temperature (T_P) and heat of fusion (ΔH_f) can be used as parameters for optimizing the DSC performance. Two model pharmaceuticals acetaminophen and nicotinamide are used in this study. Using a factorial design for the experimental model and matrix analysis the results, the effect of sample mass, heating rate and the nitrogen flow rate were evaluated on the ΔH_f values and T_P values. Two levels for each of the procedural variables were used as a balanced experimental design with two sample sizes, two heating rates and two nitrogen flow rates. It was found that the change in the heating rate caused significant changes in the ΔH_f values but not the T_p values for acetaminophen. However, no significant effect was found for the T_p value but ΔH_f value was affected to a certain extent for nicotinamide.