Dual catalytic performance of arene-ruthenium amine complexes for norbornene ring-opening metathesis and methyl methacrylate atom-transfer radical polymerizations

Arene ruthenium(II) complexes bearing the cyclic amines RuCl₂(η⁶-p-cymene)(pyrrolidine)] ( 1 ), [RuCl₂(η⁶-p-cymene)(piperidine)] ( 2 ), and [RuCl₂(η⁶-p-cymene)(peridroazepine)] ( 3 ) were successfully synthesized. Complexes 1 – 3 were fully characterized by means of Fourier transform infrared, UV–visible, and NMR spectroscopy, elemental analysis, cyclic voltammetry, computational methods, and one of the complexes was further studied by single crystal X-ray crystallography. These compounds were evaluated as catalytic precursors for ring-opening metathesis polymerization (ROMP) of norbornene (NBE) and atom-transfer radical polymerization (ATRP) of methyl methacrylate (MMA). NBE polymerization via ROMP was evaluated using complexes 1 – 3 as precatalysts in the presence of ethyl diazoacetate (EDA) under different [NBE]/[EDA]/[Ru] ratios, temperatures (25 and 50°C), and reaction times (5–60 min). The highest yields of polyNBE were obtained with [NBE]/[EDA]/[Ru] = 5000/28/1 for 60 min at 50°C. MMA polymerization via ATRP was conducted using 1 – 3 as catalysts in the presence of ethyl-α-bromoisobutyrate (EBiB) as initiator. The catalytic tests were evaluated as a function of the reaction time using the initial molar ratio of [MMA]/[EBiB]/[Ru] = 1000/2/1 at 95°C. The increase in molecular weight as function of time indicates that complexes 1–3 were able to mediate the MMA polymerization with an acceptable rate and some level of control. Differences in the rate of polymerization were observed in the order 3 > 2 > 1 for the ROMP and ATRP.     

QSAR modelling and structural aspects concerning synthetic heterocycles with larvicidal activity against Aedes aegypti

Structural Chemistry - In this paper, we present a quantitative structure–activity relationships modelling for two series of heterocyclic synthetic compounds with larvicidal activity against...     

Newton–Okounkov bodies on projective bundles over curves

Mathematische Zeitschrift - In this article, we study Newton–Okounkov bodies on projective vector bundles over curves. Inspired by Wolfe’s estimates used to compute the volume function...     

Compactness Results for a Class of Limiting Interpolation Methods

We study the behavior of compact operators when we interpolate them by real methods defined through slowly varying functions and rearrangement invariant spaces. We apply these results to prove compactness of certain integral operators acting between grand Lebesgue spaces and between small Lebesgue spaces.

     

Determination of mazindol in human oral fluid by high performance liquid chromatography–electrospray ionization mass spectrometry

Brazil is one of the countries most affected by abuse of stimulant medications by professional drivers, especially fenproporex, amfepramone and mazindol. Even though their sale is banned, they can be found in illegal markets, such as those located on the country's borders. The use of oral fluid to monitor drug levels has many advantages over plasma and urine because it is noninvasive, easier to collect and more difficult to adulterate. The aim of this study was to develop and validate a sensitive and specific method to quantify mazindol in human oral fluid by liquid chromatography–mass spectrometry (LC‐MS). The LC system consisted of an LC‐MS system operated in selected ion monitoring mode. The mobile phase was composed of water at pH 4.0, acetonitrile and methanol (60:15:25 v/v/v) at a flow rate of 1.0 mL/min and propranolol was used as internal standard. Total running time was 10 min. The lower limit of quantification was 0.2 ng/mL and the method exhibited good linearity within the 0.2–20 ng/mL range (r = 0.9987). A rapid, specific, sensitive, linear, precise and accurate method was developed for determination of mazindol in human oral fluid according to European Medicines Agency guidelines, and is suitable for monitoring mazindol levels in oral fluid of professional drivers. Copyright © 2014 John Wiley & Sons, Ltd.     

Synthesis of α-alkenyl-α-amino esters via addition of potassium Alkenyltrifluoroborate salts to imine in the presence of Yb(OTf)3

A simple protocol which led to an effective construction of α-alkenyl-α-amino esters was achieved under mild conditions. This transformation proceeded by Yb-catalyzed addition of alkenyltrifluoroborates across the imine double bond. A variety of functional groups could be applicable to both partners.