4‐Benzoyl‐3,4‐dihydro‐2H‐1,4‐benzoxazine‐2‐carbonitrile: refinement using a multipolar atom model

The structural model for the title compound, C₁₆H₁₂N₂O₂, was refined using a multipolar atom model transferred from an experimental electron‐density database. The refinement showed some improvements of crystallographic statistical indices when compared with a conventional spherical neutral‐atom refinement. The title compound adopts a half‐chair conformation. The amide N atom lies almost in the plane defined by the three neighbouring C atoms. In the crystal structure, molecules are linked by weak intermolecular C—H...O and C—H...π hydrogen bonds.     

Uncertainty calculations in the certification of reference materials

To serve as a measurement standard, a (certified) reference material must be stable. For this purpose, the material should undergo stability testing after it has been prepared. This paper looks at the statistical aspects of stability testing. Essentially, these studies can be described with analysis of variance statistics, including variant regression analysis. The latter is used in practice for both trend analysis and for the development of expressions for extrapolations. Extrapolation of stability data is briefly touched upon, as far as the combined standard uncertainty of the reference material is concerned. There are different options to validate the extrapolations made from initial stability studies, and some of them might influence the uncertainty of the reference material and/or the shelf-life. The latter is the more commonly observed consequence of what is called ’stability monitoring’. Received: 6 October 2000 Accepted: 4 December 2000     

Solvent-free synthesis of nitrones in a ball-mill

Various C-aryl and C-alkyl-nitrones were synthesized within 0.5–2 h via condensation of an equimolar amount of aldehydes and N-substituted-hydroxylamines under solvent-free conditions in a ball-mill apparatus. Reactions can be performed without the need of excluding air and moisture and yields the expected products with no need for further purification. The study has been complemented by Differential Scanning Calorimetry (DSC) and solid-state ¹³C MAS nuclear magnetic resonance experiments. We have also studied the temperature profile during the reaction. A comparative study with the corresponding solvent-free microwave activated reaction showed the superiority of the ball-milling method; 31 examples are described, including the synthesis of the anti-aging agent C-phenyl-N-tert-butyl nitrone (PBN) and one of its analogues C-2-pyridyl-N-tert-butylnitrone (2-PyBN).     

The excess intersection formula for Grothendieck–Witt groups

We prove the excess intersection and self intersection formulae for Grothendieck–Witt groups.     

An efficient route to a 5,6-dihydropyrano[3,4-b]pyridin-8-one core in two steps from enaminolactones

A convenient two step conversion of heterocyclic enaminolactones to heterocyclic fused 2-pyran-1-ones is reported. The use of this method can be applied to a wide variety of aromatic and heteroaromatic amines to give potentially biologically active compounds in good yields.