Low temperature fluorination of sulphur compounds with elemental fluorine

Low temperature fluorination technique is adopted for fluorination of the following sulphur compounds in freon-11 medium (1) Sulphur dioxide (2) Thionyl chloride (3) Sulphuryl chloride (4) Tetrasulphur tetra nitride and (5) Sulphur bromide. All the compounds undergo oxidative fluorination to give rise to sulphur-fluorine compounds except sulphuryl chloride which resists fluorination. Sulphuryl chloride thus behaves as a good solvent medium for fluorination of other reactive compounds like elemental sulphur. Details of the experimental procedures adopted and the identification of the products will be presented.     

NOVEL THREE COMPONENT SYNTHESIS OF 1,2,4-TRIAZOLO[3,4-b]THIAZOLES AND THEIR ANTIMICROBIAL ACTIVITY

1,2,4-Triazolo[3,4-b]thiazole derivatives 5a–j have been synthesized by novel multi-component reaction of 2,4-dichloro-5-fluorophenacyl bromide (1), thiosemicarbazide (2), and aromatic carboxylic acids (4) using phosphorous oxychloride as the cyclizing agent. This reaction protocol is simple, efficient, and requires shorter reaction times in comparison to the conventional multi-step synthesis. The products were identified to be same by an alternate synthesis. All the compounds were screened for their antimicrobial activity against some of bacterial and fungal strains.     

Two New Pseudoguaianolides from the Flowers of Parthenium hysterophorus

Chemical investigation on two samples of the flowers of Parthenium hysterophorus afforded two new pseudoguaianolides (one from each sample) together with several known constituents. The structures of the new compounds were established by extensive spectroscopic (1D‐ and 2D‐NMR) studies. The X‐ray crystallographic analysis of one of these compounds was also accomplished.     

Studies in the hydrolysis of metal ions

The hydrolysis of cupric ion has been studied at various ionic strengths (0·01, 0·05, 0·1 and 0·5 M). The results are analyzed employing ‘core + links’ theory, log-log plot, normalization plot, and extrapolation method for obtaining the pure mononuclear curve. The stability constants of Cu₂(OH) ₂ ⁺⁺ , Cu₃(OH) ₄ ⁺⁺ , Cu(OH)⁺ and Cu(OH)₂ have been reported.     

Spectrophotometric and potentiometric investigations of copper (II)-Ethanolamine complexes

Spectrophotometric and potentiometric investigations have been carried out on copper-diethanolamine system. Job plots at 900, 900 and 580 mμ have indicated the formation of CuD⁺⁺, CuD₂ ⁺⁺ and CuD₃ ⁺⁺. Then- pA curves obtained indicate the formation of CuD⁺⁺, CuD₂ ⁺⁺, CuD₃ ⁺⁺, CuDOH⁺, CuD₂OH⁺ and CuD₃OH⁺. Then- pA curves have been analyzed to obtain the stability constants of these complexes. Absorption curves of pure complexes have been computed by a graphical method. Gaussian analysis of the absorption curves of pure and hydroxy complexes show the presence of a second band, indicating that the structure is that of a distorted octahedron.     

Reaction of sulphuryl chlorofluoride with a few metals and metal oxides

Sulphuryl chlorofluoride has no observable reaction with metals and metal oxides at room temperature. Metals like copper, silver, iron, and zinc react with the chlorofluoride in the temperature range 200–400°C. Metal chlorides, metal fluorides and sulphur dioxide are the main products of these reactions. With the corresponding metal oxides, on the other hand, the respective metal sulphates are formed in addition to the metal chlorides and fluorides. In the case of lead and lead oxide, lead chlorofluoride is formed instead of lead chloride and lead fluoride. Sulphuryl fluoride is formed in small quantities in all these reactions by the decomposition of the chlorofluoride. Glass is not attacked by sulphuryl chlorofluoride below 500°C.During the course of our investigations on the reactivity of sulphuryl chlorofluoride, it is observed that sulphuryl chlorofluoride does not react with glass up to 500° C. However, it reacts with metals and metal oxides between 200° to 400° C. The reaction products with metals are the corresponding metal chlorides, metal fluorides and sulphur dioxide. With the oxides, in addition to the metal chlorides and metal fluorides, metal sulphates are formed. The results of these investigations are presented in this communication.     

Redox indicators in titrations with dichloramine-B

Naphthidine, dimethylnaphthidine, dimethylnaphthidinedisulphonic acid, o-dianisidine, Quinoline Yellow, diphenylbenzidine and Amaranth are proposed as indicators in titrations of arsenic(III), iron(II), antimony(III), hydroquinone, hydrazinium sulphate, phenylhydrazine hydrochloride, semicarbazide hydrochloride and ascorbic acid with dichloramine-B. They give a very sharp colour change at the equivalence point. Arsenic(III) and iron(II) are suggested for standardization of dichloramine-B solutions. A potentiometric method for the determination of arsenic(III) and semicarbazide hydrochloride is described.     

Reactions of sulphuryl fluoride,sulphuryl chlorofluoride and sulphuryl chloride with amines

The reactions of sulphuryl fluoride, sulphuryl chlorofluoride and sulphuryl chloride with the amines tert-butylamine, benzylamine, piperidine, pyridine and quinoline have been investigated. The primary and secondary amines react with the elimination of hydrogen halides and formation of SN bonds whereas tertiary amines form 1:2 adducts.     

Metabolite Dysregulation by Pranlukast in Mycobacterium tuberculosis

Mycobacterium tuberculosis has been infecting millions of people worldwide over the years, causing tuberculosis. Drugs targeting distinct cellular mechanisms including synthesis of the cell wall, lipids, proteins, and nucleic acids in Mtb are currently being used for the treatment of TB. Although extensive research is being carried out at the molecular level in the infected host and pathogen, the identification of suitable drug targets and drugs remains under explored. Pranlukast, an allosteric inhibitor of MtArgJ (Mtb ornithine acetyltransferase) has previously been shown to inhibit the survival and virulence of Mtb. The main objective of this study was to identify the altered metabolic pathways and biological processes associated with the differentially expressed metabolites by PRK in Mtb. Here in this study, metabolomics was carried out using an LC-MS/MS-based approach. Collectively, 50 metabolites were identified to be differentially expressed with a significant p-value through a global metabolomic approach using a high-resolution mass spectrometer. Metabolites downstream of argJ were downregulated in the arginine biosynthetic pathway following pranlukast treatment. Predicted human protein interactors of pranlukast-treated Mtb metabolome were identified in association with autophagy, inflammation, DNA repair, and other immune-related processes. Further metabolites including N-acetylglutamate, argininosuccinate, L-arginine, succinate, ergothioneine, and L-phenylalanine were validated by multiple reaction monitoring, a targeted mass spectrometry-based metabolomic approach. This study facilitates the understanding of pranlukast-mediated metabolic changes in Mtb and holds the potential to identify novel therapeutic approaches using metabolic pathways in Mtb.