The crystal and molecular structure of 2,7-diazanaphthalene

X-ray diffraction data were collected at 20°C on a computer-controlled Philips diffractometer (PW 1100). The structure was solved by direct methods and refined by the full-matrix least-squares method to an R of 0.065 (weighted R 0.046). The molecule in the crystal is of lower symmetry than C2,.. The geometry of the molecule has been compared with NMR results obtained by Danieli, Lunazzi & Veracini [J. Chem. Soc. Perkin II, (1976), pp. 19-201. As a result a C-H bond-length correction of 0.09 (2) A was found

1,4-diacetoxy-β-lactams. Reactions with nucleophiles

β-Lactam reacts with hetero nucleophiles under ring cleavage to give 2,2-dimethyl-3-oximinobutanoic esters 6 and 7 . N-hydroxyazetidine 5 , the precursor of β-lactam 1, is prepared by a new method

A correction procedure for the errors in single-crystal intensities due to the inhomogeneity of the primary X-ray beam

Graphite monochromators are known to give rise to non-homogeneous primary X-ray beams. When intensities of single crystals are measured the effective cross section of a non-spherical crystal in the X-ray beam depends on its orientation in the beam. Therefore, systematic errors in the measured integrated intensities are introduced by the inhomogeneity of the incoming beam. A correction for these errors can be made, knowing the intensity profile of the primary beam and the dimensions and orientation of the crystal in the beam. The correction can conveniently be applied with the absorption correction. Examples of the corrections are given for crystals with rational boundary planes. It is shown that the intensity of an X-ray reflection as a function of the rotation about the scattering vector ( rotation) can be calculated with fair accuracy. In some cases (large elongated crystals in an inhomogeneous beam) correction for absorption only may give results which are worse than those with no correction at all

Novel applications of the “t-amino effect” in heterocyclic chemistry; synthesis of 1-alkylindoles

Thermal rearrangerment of 2-vinyl-1-(1-pyrrolidinyl)benzenes varies with the leaving group ability of substituents in the vinyl moiety; compound 3 having an OR group 9-(alkoxy-methyl)pyrrolo[1,2-a]indoles and compounds 6 (X = OAc, OTs or Cl) yield 1-alkylindoles

Synthesis of pyrrolizines by intramolecular capture of 1,4-dipolar intermediates in reactions of enamines with dimethyl acetylenedicarboxylate

Solvent polarity and reaction temperature strongly influence the reactions of dimethyl acetylenedicar-boxylate (DMAD) with 1-pyrrolidinyl enamines of acyclic and cyclic ketones. Whereas DMAD and 1-[1-phenyl-2-(phenylthio)ethenyl]pyrrolidine (3) give only a mixture of the isomeric 1,3-butadienes (5) in apolar solvents, in methanol the main product is the pyrrolizine 7, together with 5. Again in methanol, DMAD reacts at 0-5° with 8, 9 and 10 to give exclusively 1:1 adducts, the pyrrolizines 11,12 and 13, respectively, whereas at −50° 8 and 9 give 1:2 (enamine : DMAD) adducts, the pyrrolizines 14 and 15, respectively; a single crystal X-ray analysis of 14 gave the structure of the 1:2 adducts. In the same solvent methyl propiolate and 8 give only the linear Michael adduct 17. The enamine-ketone 18 reacts with DMAD in propylene carbonate at 0–5° to give, via (2 + 2)-cycloaddition and ring expansion, 19, and the linear Michael adduct 20. The mechanism of (2 + 2)-cycloaddition and pyrrolizine formation is discussed in terms of a common tied-ion pair intermediate formed in the first, rate-determining step, followed by a second solvent-dependent step

Using the analytic hierarchy process to support teams in defining new product objectives

Defining new product objectives is a critical problem solving activity to new product success. The analytic hierarchy process appears to be an adequate technique for multi-criteria decision analysis to support the definition of new product objectives. To illustrate this support, we applied this technique to a project focused on the development of a liver perfusion system to preserve donor livers. It quantitatively supported discussions between technological developers and clinical practitioners focused on the product requirements and the pursued performance of the liver perfusion system relative to an envisaged competitor. The discussions significantly reduced disagreements about the new product objectives between the group members. They resulted in a quantitative overview of the importance of the product requirements and the relative performance of the alternatives with regard to these requirements. Furthermore, research activities necessary to fulfil these objectives were discerned. The group members were committed to these outcomes. This application shows the value of introducing the AHP as a means to steer new products to solve problems to a higher extent than competing products do

The atomic surface structure of SrTiO3 (001) studied with synchrotron X-rays

The atomic surface structure of single terminated SrTiO3(0 0 1) (1 × 1) is investigated employing surface X-ray diffraction. In order to obtain these surfaces a special treatment is needed consisting of chemical etching and annealing. Since this is done in an aqueous and subsequently oxygen environment, after which the crystals are kept at ambient conditions, the surface is studied in air. Crystal truncation rods are measured and several models that are proposed in literature in recent years are tested against the experimental data. These models include surface rumpling, low temperature-like distortions, strontium adatom and lateral displacement distortions for both TiO2 and SrO-terminated surfaces. None of these models represents the data very accurately. A much better fit to the experimental results is obtained by using a model in which a TiO2-terminated crystal is covered by an oxygen layer

Reduction of nitro groups by ynamines; synthesis and x-ray crystal structure of n,n-diethyl-3,3a-dihydro-3-methylbenzofuro[3,2-c]isoxazole-3-carboxamide

3-Nitrobenzo[b]furan and 1-diethylaminopropyne react thermally at 5–10°C to give a 1:1 addition product ( ) in which one of the oxygen atoms of the nitro group is transferred to C-1 of the acetylene. The structure of the benzofuro[3,2-c]isoxazole ( ) has been determined by X-ray crystallography