Far infrared spectra of solid molecular nitrogen

This paper reports the observation of the far infrared absorption spectrum of a single crystal of N₂, measured over absorption paths of 4 cm (lengthwise) and 2 cm (across the crystal). The crystal chamber, with quartz windows, was immersed in a flow of cold helium gas. The spectrum from 20 to 120 cm^–1 was recorded in the liquid phase, the-phase, and over the full temperature range of the-phase (35.6–2.0 K) with a Fourier transform spectrometer. The spectral resolution, which was not instrument-limited, and the large path allowed the observation of more detailed multiphonon-transition structure in the spectrum of the-phase than has previously been observed.     

Serendipitous synthesis of a ditwistane: a one-step access!

4-tert-Butyl-2-cyclohexen-1-one dimerizes in THF solution via its kinetic enolate, leading to di-tert-butylditwistane 8 in up to 36% yield (−78 °C → room temp., protonolysis, flash chromatography). X-ray crystallography shows that 8 incorporates one R and one S enantiomer of the starting ketone; none of the diastereomeric ditwistanes epi-8, epi’-8 or iso-8 was isolated. This means that the formation of 8 proceeds with mutual kinetic resolution and 100% induced diastereoselectivity.     

Kopsirachin,ein ungewöhnliches Alkaloid aus der Apocynaceae Kopsia dasyrachis Ridl. 189. Mitteilung über organische Naturstoffe

Kopsirachine, an Unusual Alkaloid from the Apocynaceae Kopsia dasyrachis Ridl. From the leaves of Kopsia dasyrachis Ridl. a new type of alkaloid, kopsirachine ( 1 ), built up from catechin ( 2 ) and skytanthine ( 3 ) has been isolated. The structure elucidationis based on spectral and chemical evidence. Oxidative cleavage of its derivative 4 with KMnO₄ afforded veratric acid wich was identified as its methylester by comparison with an authentic sample. Pyrolysis of 1 yielded δ-skytanthine ( 3 ). The stereochemistry of the skytanthine substituents in 1 could not yet be established.     

Notiz zur quantitativen Bestimmung von Si-H- und Si-Si-Gruppen

Zusammenfassung Eine einfache und genaue Methode zur Bestimmung von Si-H- und Si-Si-Gruppen wird vorgeschlagen, die auf alkalischer Hydrolyse der Substanz in einem verschlossenen und evakuierten Kolben und AuswÄgen des dem entwickelten Wasserstoff entsprechenden Wasservolumens beruht. Bei H-Gehalten von 1–2% betrÄgt die Genauigkeit ± 0,03% (abs.).

---

Note on the quantitative determination of Si-H- and Si-Si-groups

A simple, robust and surprisingly exact method for the quantitative determination of Si-H- or Si-Si-groups is based on alkaline hydrolysis of the Si-H- or Si-Si-containing substances in a sealed and evacuated vessel and weighing of the volume of water equivalent to the developed volume of hydrogen. The accuracy is ± 0.03% (abs.) with H contents of 1–2%.

---

---

Herrn Prof. Dr. E. Asmus zum 60. Geburtstag gewidmet.