M. Akssira

Synthesis of New Compounds Containing the 2,3-dihydro-1, 4-dioxino[2,3-b]pyridine Heterocyclic System as a Substructure:

2,3-Dihydro-spiro[1,4]dioxino[2,3-b]pyridine-3,3′-pyrrolidine (8A) and 2,3-dihydro-spiro[1,4]dioxino[2,3-b]pyridine-3,4′-piperidine (9A) have been synthesized from 2-chloro-3-pyridinol. The corresponding 2,3′ (8B) and 2,4′ (9B) isomers were obtained via the Smiles rearrangement, while 9B was also selectively synthesized from 2-nitro-3-pyridinol. The separation of the isomers A and B under the sulfamide form was carried out by flash column chromatography. Subsequent transformations of the corresponding dioxinopyridine derivatives were described.

Metal free direct formation of various substituted pyrido[2′,1′:2,3]imidazo[4,5-c]isoquinolin-5-amines and their further functionalization

Original substituted pyrido[2′,1′:2,3]imidazo[4,5-c]isoquinolin-5-amines have been prepared following a Groebke–Blackburn–Bienayme MCR combined with an N-deprotection and a spontaneous final cyclization step in moderate to good yields. The flexibility of the described method enables the introduction of diverse groups in the 6 and 7 positions on the resulting scaffold using commercially available starting materials. Furthermore, a Buchwald–Hartwig cross coupling with a wide range of aryl and hetaryl halides has been successfully reported using our heterocyclic primary amine derivatives.

Comparative Study of Retention of Glucosinolates and Inorganic Ions on Selected Silica‐Based and Polymer‐Based Ion Exchange Columns

Abstract The retention of two glucosinolates [Sinigrin (SIN), Glucotropaeolin (GTL)] and oxalate as organic anions and inorganic anions (chloride, nitrate, sulfate) were studied on three anion exchangers, e.g., Vydac 302 IC (250 × 4.6 mm I.D.), Dionex Ion Pac (250 × 4 mm I.D.), and Waters IC Pac HR (75 × 4.6 mm I.D.) under isocratic elution conditions. The two glucosinolates carry the same functional group (‒OSO3 −), however, do not have the same retention in anion exchange chromatography. The plots of capacity factors k of organic and inorganic anions vs. the reciprocal of eluent ion concentration show good linearity. From the slope and y‐intercept data, the major retention mechanisms are interpreted as ion exchange and some other interactions. The influence of organic modifier addition to the aqueous buffered mobile phase is also investigated. An Evaporative Light Scattering Detector (ELSD) was used.

Fe–Cu catalyzed synthesis of symmetrical and unsymmetrical diaryl thioethers using 1,3-benzoxazole-2-thiol as a sulfur surrogate

An efficient Fe–Cu catalyzed approach is herein developed using 1,3-benzoxazole-2-thiol as a thiol surrogate for the synthesis of symmetrical and unsymmetrical diaryl thioethers. This method provides an odorless and inexpensive strategy which can be applied to various aryl and nitrogen containing aryl halides in moderate to excellent yields up to 90%.

Synthetic Modification of 9α- and 9β-Hydroxyparthenolide by Heck or Acylation Reactions and Evaluation of Cytotoxic Activities

Motivated by the widely reported anticancer activity of parthenolides and their derivatives, a series of new substituted parthenolides was efficiently synthesized. Structural modifications were performed at the C-9 and C-13 positions of 9α- and 9β-hydroxyparthenolide, which were isolated from the aerial parts of Anvillea radiata. Twenty-one derivatives were synthesized and evaluated for their in vitro cytotoxic activity against HS-683, SK-MEL-28, A549, and MCF-7 human cancer cell lines using the MTT colorimetric assay. Among the derivatives, seven exhibited excellent activity compared to 5-fluorouracil and etoposide against the four cell lines tested, with IC50 values ranging from 1.1 to 9.4u2009µM.

New Approach for Inorganic Anion Analysis by Ion Exchange Chromatography Coupled with Evaporative Light Scattering Detection

Abstract The simultaneous separation of inorganic anions is possible by ion exchange chromatography (IEC) under an isocratic elution mode, using polymer exchanger Metrosep anion dual1 Metrohm (150 × 3 mm ID) followed by evaporative light scattering detection (ELSD). Several mobile phases [formic acid (FA)/ammonia, FA, hydrogen carbonate, trifluoro‐acetic acid (TFA), and heptafluorobutyric acid (HFBA)] were tested for optimization of the separation of inorganic anions. The choice of a mobile phase was proven by compatibility with ELSD volatility requirements.