Preparation of 1,5-methano-2,3,4,5- tetrahydro-1H-3-benzazepine via Pd-catalyzed cyclization

[reaction: see text] A new approach to prepare 1,5-methano-2,3,4,5-tetrahydro-1H-3-benzanepine (1) is discussed. This strategy utilized a tandem Michael addition and Pd-catalyzed cyclization to afford cyanobenzofulvene acetal 13. This indene intermediate (13) was subjected to hydrogenolysis to provide an amino ester (12) and was cyclized with base to afford lactam 5. The lactam (5) was reduced with borane to afford the desired benzazepine (1).     

Coupling miniaturized liquid chromatography to capillary gas chromatography (micro-LC-CGC): Possibilities of reversed phase LC

Retention gaps with different polarity treatments were evaluated for reversed phase solvents. Aminopropyl- and cyanopropyl-deactivated retention gaps showed the best results for methanol-water mixtures. A reversed phase packed fused silica capillary LC column is connected on-line with a capillary gas chromatography column. The combination was used for the analysis of diazepam in urine. Volume overloading on packed fused silica columns without loss of too much efficiency was demonstrated for propranolol.     

Effect of Particle Size on the Photocatalytic Activity of Nanoparticulate Zinc Oxide

In this study, a three-stage process consisting of mechanical milling, heat treatment, and washing has been used to manufacture nanoparticulate ZnO powders with a controlled particle size and minimal agglomeration. By varying the temperature of the post-milling heat treatment, it was possible to control the average particle size over the range of 28–57 nm. The photocatalytic activity of these powders was characterized by measuring the hydroxyl radical concentration as a function of irradiation time using the spin-trapping technique with electron paramagnetic resonance spectroscopy. It was found that there exists an optimum particle size of approximately 33 nm for which the photocatalytic activity is maximized. The existence of this optimal particle size is attributable to an increase in the charge carrier recombination rate, which counteracts the increased activity arising from the higher specific surface area for a sufficiently small particle size.     

A comparative evaluation of the photocatalytic and optical properties of nanoparticulate ZnO synthesised by mechanochemical processing

In this study, mechanochemical processing has been used to manufacture a nanoparticulate powder of ZnO with a controlled particle size and minimal hard agglomeration. The suitability of this ZnO powder for use as either a photocatalyst or an optically transparent UV-filter was evaluated by comparing its optical and photocatalytic properties with those of three commercially available powders that were synthesised by chemical precipitation and flame pyrolysis. The ZnO powder synthesised by mechanochemical processing was found to exhibit high optical transparency and low photocatalytic activity per unit of surface area, which indicates that it is suitable for use in optically transparent UV-filters.

     

Efficient delivery of Cre-recombinase to neurons in vivo and stable transduction of neurons using adeno-associated and lentiviral vectors

Background

As development proceeds the human embryo attains an ever more complex three dimensional (3D) structure. Analyzing the gene expression patterns that underlie these changes and interpreting their significance depends on identifying the anatomical structures to which they map and following these patterns in developing 3D structures over time. The difficulty of this task greatly increases as more gene expression patterns are added, particularly in organs with complex 3D structures such as the brain. Optical Projection Tomography (OPT) is a new technology which has been developed for rapidly generating digital 3D models of intact specimens. We have assessed the resolution of unstained neuronal structures within a Carnegie Stage (CS)17 OPT model and tested its use as a framework onto which anatomical structures can be defined and gene expression data mapped.

Results

Resolution of the OPT models was assessed by comparison of digital sections with physical sections stained, either with haematoxylin and eosin (H&E) or by immunocytochemistry for GAP43 or PAX6, to identify specific anatomical features. Despite the 3D models being of unstained tissue, peripheral nervous system structures from the trigeminal ganglion (~300 μm by ~150 μm) to the rootlets of cranial nerve XII (~20 μm in diameter) were clearly identifiable, as were structures in the developing neural tube such as the zona limitans intrathalamica (core is ~30 μm thick). Fourteen anatomical domains have been identified and visualised within the CS17 model. Two 3D gene expression domains, known to be defined by Pax6 expression in the mouse, were clearly visible when PAX6 data from 2D sections were mapped to the CS17 model. The feasibility of applying the OPT technology to all stages from CS12 to CS23, which encompasses the major period of organogenesis for the human developing central nervous system, was successfully demonstrated.

Conclusion

In the CS17 model considerable detail is visible within the developing nervous system at a minimum resolution of ~20 μm and 3D anatomical and gene expression domains can be defined and visualised successfully. The OPT models and accompanying technologies for manipulating them provide a powerful approach to visualising and analysing gene expression and morphology during early human brain development.     

Preparation of polystyrene with long chain branches via free radical polymerization

Polystyrene with random long chain branches has been difficult to prepare. A new approach using small amounts of chain-transferring monomers to copolymerize with styrene free radically was examined in this work. Of the several comonomers examined, vinylbenzylthiol yielded polystyrene with branched structure. But because of the high chain trnsfer constant, the branches occurred mainly in the low-molecular-weight end of the distribution. As a side interest, vinylbenzylthiol was found to be an effective agent for the broadening of molecular weight distribution.     

High shear rate viscometry

We investigate the use of two distinct and complementary approaches in measuring the viscometric properties of low viscosity complex fluids at high shear rates up to 80,000 s^?1. Firstly, we adapt commercial controlled-stress and controlled-rate rheometers to access elevated shear rates by using parallel-plate fixtures with very small gap settings (down to 30 μm). The resulting apparent viscosities are gap dependent and systematically in error, but the data can be corrected—at least for Newtonian fluids—via a simple linear gap correction originally presented by Connelly and Greener, J. Rheol, 29(2):209–226, 1985). Secondly, we use a microfabricated rheometer-on-a-chip to measure the steady flow curve in rectangular microchannels. The Weissenberg–Rabinowitsch–Mooney analysis is used to convert measurements of the pressure-drop/flow-rate relationship into the true wall-shear rate and the corresponding rate-dependent viscosity. Microchannel measurements are presented for a range of Newtonian calibration oils, a weakly shear-thinning dilute solution of poly(ethylene oxide), a strongly shear-thinning concentrated solution of xanthan gum, and a wormlike micelle solution that exhibits shear banding at a critical stress. Excellent agreement between the two approaches is obtained for the Newtonian calibration oils, and the relative benefits of each technique are compared and contrasted by considering the physical processes and instrumental limitations that bound the operating spaces for each device.