Synthesis of 1,3-dioxo-hexahydropyrido[1,2-c][1,3]diazepine carboxylates, a new bicyclic skeleton formed by ring expansion-RCM methodology

A short and elegant synthetic pathway was developed for the synthesis of 1,3-dioxo-hexahydropyrido[1,2-c][1,3]diazepine carboxylates, a new 1,3-diazepan-2,4-dione containing bicyclic moiety, starting from pyroglutamate esters.     

Using a facility location algorithm to solve large set covering problems

Erlenkotter has developed an efficient exact (guarantees optimality) algorithm to solve the uncapacitated facility location problem (UFLP). In this paper, we use his algorithm to solve large instances of an important subset of the UFLP; the set covering problem (SCP). In addition, we present further empirical evidence that a heuristic algorithm developed by Vasko and Wilson for the SCP is capable of quickly generating good solutions to large SCP's.     

Revision of an enamine synthesis; the preparation and reactions of 2-morpholinoisoflav-3-ene.

The condensation of $\text{N}$-styrylmorpholine with salicylaldehyde does $\text{not}$ give a product that can be oxidised to isoflavone; the product is $\text{N}$-morpholino-isoflav-3-ene which can be used to prepare other compounds related to isoflavan and upon oxidation gives 3-phenylcoumarin.     

Gas-Phase Enrichment of Multiply Charged Peptide Ions by Differential Ion Mobility Extend the Comprehensiveness of SUMO Proteome Analyses

The small ubiquitin-like modifier (SUMO) is a member of the family of ubiquitin-like modifiers (UBLs) and is involved in important cellular processes, including DNA damage response, meiosis and cellular trafficking. The large-scale identification of SUMO peptides in a site-specific manner is challenging not only because of the low abundance and dynamic nature of this modification, but also due to the branched structure of the corresponding peptides that further complicate their identification using conventional search engines. Here, we exploited the unusual structure of SUMO peptides to facilitate their separation by high-field asymmetric waveform ion mobility spectrometry (FAIMS) and increase the coverage of SUMO proteome analysis. Upon trypsin digestion, branched peptides contain a SUMO remnant side chain and predominantly form triply protonated ions that facilitate their gas-phase separation using FAIMS. We evaluated the mobility characteristics of synthetic SUMO peptides and further demonstrated the application of FAIMS to profile the changes in protein SUMOylation of HEK293 cells following heat shock, a condition known to affect this modification. FAIMS typically provided a 10-fold improvement of detection limit of SUMO peptides, and enabled a 36% increase in SUMO proteome coverage compared to the same LC-MS/MS analyses performed without FAIMS.

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A method for visualization of ventricular fibrillation: Design of a cooled fiberoptically coupled image intensified CCD data acquisition system incorporating wavelet shrinkage based adaptive filtering

The measurement of cardiac transmembrane potential changes with voltage sensitive dyes is in increasing use. Detection of these very small fluorescent alterations using large multiplexed arrays, such as charge coupled device (CCD) cameras at high sampling rates, has proven challenging and usually requires significant averaging to improve the signal-to-noise ratio. To minimize the damage of living tissue stained with voltage sensitive dyes, excitation photon exposure must be limited, with the inevitable consequence of diminishing the fluorescence that is generated. State-of-the-art high frame rate CCD cameras have read noise levels in the 5-10 e(-) rms range, which is at least two orders of magnitude above that required to detect voltage sensitive dye alterations at individual pixels corresponding to 1 mm(2) heart regions illuminated with levels of 100 mW/cm(2) at frame rates approaching 1000 frames/sec. Image intensification is thus required prior to photon quantification. We report here the development of such a data acquisition system using commercially available hardware. Additionally, in the past ten years, a mathematical theory of multiresolution has been developed, and new building blocks called wavelets, allow a signal to be observed at different resolutions. Wavelet analysis also makes possible a new method of extricating signals from noise. We have incorporated spatially adaptive filters based on wavelet denoising of individual pixels to significantly reduce the multiple noise sources present in the acquired data. (c) 1998 American Institute of Physics.     

X-ray structure of sesterterpene, 16β-acetoxy-24-methyl-12,24-dioxoscalaran-25-al

The molecular geometry of a tetracyclic sesterterpene has been determined by X-ray diffraction. The conformation of the aldehyde group as observed in the crystal structure supports the rationalization for the absence of aldehyde proton coupling in the nmr spectra of the compound. Crystal data: C₂₈H₄₂O₅, M.W.=458.6; orthorhombic, P2₁2₁2₁;a=10.797(2),b=29.270(9),c=8.033(1)Å,V=2538.7ų,Dx=1.199 g cm^–3;R=0.045 for 2287 observed reflections.