A Validated Chiral LC Method for the Determination of Enantiomeric Purity of Pemetrexed Disodium on an Amylose-Based Chiral Stationary Phase

A simple and new isocratic normal phase chiral HPLC method has been developed for the determination of enantiomeric purity of pemetrexed disodium (l-enantiomer) in bulk drugs with a short run time of about 20 min. Chromatographic separation of l and d-enantiomers of pemetrexed disodium was achieved on an amylose based chiral stationary phase using a mobile phase consists of hexane, ethanol and trifluoro acetic acid. The resolution between the enantiomers was found to be more than 2.0. The system precision and method precision were found to be within 5% RSD for the distomer (d-enantiomer) at its specification level (i.e. not more than 1.0% w/w). The limit of detection and limit of quantification of distomer were 1.6 and 5 μg mL⁻¹, respectively for 10 μL injection volume. The percentage recovery of distomer was ranged from 90.6 to 105.7 in bulk drug samples. The test solution was found to be stable in the diluent for 48 h. The method was found to be specific for the enantiomers of pemetrexed disodium and can be conveniently used for the quantification of undesired d-enantiomer present in the bulk drug samples of pemetrexed disodium.     

Liquid Phase Regioselective Bromination of Aromatic Compounds Over Hzsm-5 Catalyst

A simple, efficient, regioselective and environmentally safe method for oxybromination of activated aromatics catalyzed by HZSM-5 is reported. The electrophilic substitution of bromine generated from KBr using HZSM-5 as a catalyst and H₂O₂ as an oxidant.     

TRANSITION METAL,NON-METAL CARBONYL CLUSTRS AS SUPPORTS FOR UNUSUAL ACETYLIDE REACTIVITY

Group 16 elements serve as useful bridging and stabilising single atom ligands in mixed-metal carbonyl complexes and impart unusual reactivity on coordinated acetylenic moieties. Reactions of [Fe ₃ (CO) ₉ (μ ₃ -E) ₂ ] (E = S, or Se) with mononuclear acetylide complexes, [CpM(CO)_3-x(CCR)] (M = Mo or W, x = 0, R = Ph; M = Fe, x = 1, R = Ph or ferrocenyl) under facile conditions yield complexes featuring acetylide coupling, acetylide-flip and formation of oxo and acetylide-bridged complexes. In presence of free acetylenes, unusual ligand systems arising from C─S bond formation are observed and under certain conditions, formation of quinones by coupling of acetylenes with carbon monoxide is facilitated.     

Development of Polar Organic Mode Chromatographic Method by Polysaccharide-Based Immobilized Chiral Selector and Validation for the Determination of the Enantiopurity of Novel Mineralocorticoid Receptor Antagonist Atropisomer–Esaxerenone

Esaxerenone is a new nonsteroidal mineralocorticoid receptor antagonist utilized to treat high blood pressure. Chemically, esaxerenone is a pyrrole derivative consisting of hindered rotation, which results in stereoisomers named atropisomers. Currently, no methods exist for the separation and quantification of these atropisomers. A new and accurate chiral liquid chromatographic technique was developed and validated to estimate the enantiomeric purity of esaxerenone. Polar organic chiral separation was carried out on an immobilized amylose-based chiral stationary phase (Chiralpak IG) with methanol:acetonitrile:diethylamine (9:1:0.1, v/v/v) mixture as a mobile phase. The total runtime was 15 min, and the resolution (R_s) between the atropisomers was more than 3.0. The detection and quantification thresholds for the R-atropisomer were found to be 0.03 and 0.1 µg mL^?1, respectively, for a test concentration of esaxerenone (1000 µg mL^?1). Over the range from the limit of quantification to 0.3 percent, the method's linearity for the R-atropisomer was excellent (R²?>?0.999). The R-atropisomer recovery varied from 95 to 102%, confirming the method’s good accuracy. For a 48-h research period, the chemical was shown to be stable.

     

A convenient new and efficient commercial synthetic route for dasatinib (Sprycel®)

A new and efficient synthetic route for dual-Src/Abl kinase inhibitor dasatinib (Sprycel®), an anticancer drug, is described. This commercially viable process yields dasatinib monohydrate free of potential impurities with consistent yield of 68% in route A and 61% in route B with HPLC purity >99.80% over four stages.     

Excess parameters of binary mixtures of anisaldehyde with o-cresol,m-cresol and p-cresol at T = (303.15, 308.15, 313.15, and 318.15) K

The density, ultrasonic velocity, and viscosity of binary mixtures of (anisaldehyde + o-cresol, or +m-cresol, or +p-cresol) have been measured over the entire range of composition at T = (303.15, 308.15, 313.15, and 318.15) K. Using these data, various thermo-acoustic parameters such as deviation in adiabatic compressibility, Δβ, excess molar volume, V^E, viscosity deviation, Δη and excess Gibb’s free energy of activation for viscous flow, ΔG^1E have been calculated. The calculated deviation and excess functions have been fitted to the Redlich–Kister polynomial equation. The negative and positive values of deviation or excess thermo-acoustic parameters observed have been explained on the basis of the intermolecular interactions present in these mixtures.     

Practical synthesis of 2-keto-3-deoxy-D-glycero-D-galactononulosonic acid (KDN)

Reaction of propargylmagnesium bromide with 2,3;5,6-di-O-isopropylidene-D-mannonolactone followed by highly stereoselective reduction of the so-formed lactol with sodium borohydride gives a syn-diol from which practical syntheses of 2-keto-3-deoxy-D-glycero-D-galactononulosonic acid (KDN) and various partially protected derivatives have been achieved all of which feature the oxidative unmasking of the α-keto acid moiety from the alkyne.     

Synthesis and Antimicrobial Activity of 1-Aryl-4-(arylimino)-6-iminohexahydro-1,3,5-triazine-2-thione Derivatives

Russian Journal of General Chemistry - A series of 6-imino-1-aryl-4-(arylimino)-1,3,5-triazinane-2-thione derivatives are synthesized by cyclization of 1-aryl-3-cyanoguanidine with aryl...