Nitrogen bridgehead compounds. Part 60. Unusual amination with sodium azide.

9-Bromo-6,7,8,9-tetrahydro-4$\text{H}$-pyrido [1,2-$\text{a}$]pyrimidin-4-ones react with sodium azide to afford 9-amino-6,7-dihydroanalogues. A mechanism involving a tricyclic tetrazine intermediate formed by neighbouring-group participation is suggested.     

Laser-polarized (129)Xe NMR and MRI at ultralow magnetic fields

Laser-polarized (129)Xe and a high-T(c)superconducting quantum interference device (SQUID) are used to obtain magnetic resonance images in porous materials at a magnetic field of 2.3 mT, corresponding to a Larmor frequency of 27 kHz. Image resolution of 1 mm is obtained with gradients of only 1 mT/m. The resolution of xenon chemical shifts in different physicochemical environments at ultralow fields is also demonstrated. Details of the circulating flow optical pumping apparatus and the SQUID spectrometer are presented.     

Ultrafast all-optical demultiplexer based on monolithic Mach–Zehnder interferometer with integrated semiconductor optical amplifiers

A monolithically integrated and fully packaged Mach–Zehnder interferometer with semiconductor optical amplifiers (MZI-SOA) is demonstrated as polarisation-independent high-speed demultiplexer for up to 160 Gbit/s optical time division multiplexed (OTDM) data streams.     

High-repetition-rate PIV investigations on a generic rocket model in sub- and supersonic flows

High-repetition-rate PIV measurements were performed in the trisonic wind tunnel facility at the Bundeswehr University Munich in order to investigate the boundary layer parameters on a generic rocket model and the recirculation area in the wake of the model at Mach numbers up to Mach = 2.6. The data are required for the validation of unsteady flow simulations. Because of the limited run time of the blow-down wind tunnel, a high-repetition-rate PIV system was applied to obtain the flow statistics with high accuracy. The results demonstrate this method’s potential to resolve small-scale flow phenomena over a wide field of view in a large Mach number range but also show its limitations for the investigations of wall-bounded flows.     

1H and 7Li NMR Study on the Complex Formation of Lithium Cations with Pyridinium Derivatives of Calix[4]arenes

Complexation of lithium ions by three chromoionophoric calix[4]arenes has been studied by ¹H and ⁷Li NMR spectroscopy. The signalling unit of the chromoionophores is the N-methylpyridinium(methyleneimino) group in conjugation with a phenolic group of the calixarene ring while the coordination spheres contain esteric (ethoxycarbonylmethoxy) or etheric (ethoxy, propoxy) units. ¹H NMR and NOESY measurements suggest the dominance of cone conformations of the calixarene rings with slight, solvent-dependent distortions. Complexation occurs only in the presence of a weak base. The interaction with lithium ions causes a broadening of both the ¹H and ⁷Li NMR signals. Analysis of the chemical shifts in the three complexes indicates a different coordination environment for the lithium with the calixarene containing esteric groups from those having etheric groups. This explains the differences in the stabilities of the lithium complexes of the two types of calixarenes.     

Unprecedented Cyclizations of Calix[4]arenes with Glycols under the Mitsunobu Protocol. Part 4. An Expedient Route to Thiacalix[4](Aza and Thia)Crowns

The Mitsunobu cyclization of p-t-butylthiacalix[4]arene with glycols was expanded to oligoethylene glycol analogues composed of O, S and N atoms in the chain. In this way a number of 1,3-thiacalix[4]monocrowns have been synthesized, offering simple and general access to a large variety of crowned thiacalixarenes. The binding properties of some ligands towards transition metal cations have been studied by ¹H NMR, UV/Vis spectroscopic and potentiometric methods.