Pd0‐Catalyzed Intramolecular α‐Arylation of Sulfones: Domino Reactions in the Synthesis of Functionalized Tetrahydroisoquinolines

A new strategy for the synthesis of tetrahydroisoquinolines based on the Pd⁰‐catalyzed intramolecular α‐arylation of sulfones is reported. The combination of this Pd‐catalyzed reaction with intermolecular Michael and aza‐Michael reactions allows the development of two‐ and three‐step domino processes to synthesize diversely functionalized scaffolds from readily available starting materials.     

Exact Max-SAT solvers for over-constrained problems

We present a new generic problem solving approach for over-constrained problems based on Max-SAT. We first define a Boolean clausal form formalism, called soft CNF formulas, that deals with blocks of clauses instead of individual clauses, and that allows one to declare each block either as hard (i.e., must be satisfied by any solution) or soft (i.e., can be violated by some solution). We then present two Max-SAT solvers that find a truth assignment that satisfies all the hard blocks of clauses and the maximum number of soft blocks of clauses. Our solvers are branch and bound algorithms equipped with original lazy data structures, powerful inference techniques, good quality lower bounds, and original variable selection heuristics. Finally, we report an experimental investigation on a representative sample of instances (random 2-SAT, Max-CSP, graph coloring, pigeon hole and quasigroup completion) which provides experimental evidence that our approach is very competitive compared with the state-of-the-art approaches developed in the CSP and SAT communities. Research partially supported by projects TIN2004-07933-C03-03 and TIC2003-00950 funded by the Ministerio de Educación y Ciencia. The second author is supported by a grant Ramón y Cajal.     

Synthesis and thermal crosslinking of oxazolidine‐functionalized polyurethanes

A new oxazolidine derivative was obtained from phenol, 2‐amino‐2‐methylpropane‐1,3‐diol and paraformaldehyde. The reaction of this novel oxazolidine diol with phenylisocyanate lead to a urethane model compound which can be polymerized thermally by oxazolidine ring opening to give a Mannich bridge structure. Linear segmented polyurethanes were prepared by reaction of different ratios of oxazolidine diol and commercial polyethylenglycol (M_w ～ 400) with 4,4′‐methylenbis (cyclohexylisocyanate) (HMDI, 90% isomers mixture). The polyurethanes were thermally characterized and crosslinked by oxazolidine ring opening to obtain materials which showed improved thermal stability. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 4965–4973, 2007     

General and selective isolation procedure for high-performance liquid chromatographic determination of anabolic steroids in tissues

A multi-residue method has been developed for the determination of anabolic steroids in animal tissue. The analytes are extracted from tissue with methanol and the extract is subjected to two solid-phase extractions, one using a non-specific adsorbing material, such as graphitized carbon black (Carbopack B), and the other Amberlite CG-400 I in the OH form. This procedure allowed the neutral anabolics (testosterone, trenbolone and progesterone) to be isolated and separated from the acidic type (phenolic group), such as diethylstilbestrol, oestradiol, zeranol/zearalenone and their respective metabolites. The determination was effected using high-performance liquid chromatography with different detectors (ultraviolet, fluorimetric and electrochemical). Several analytical parameters were studied: chromatographic conditions, recoveries, evaporation step, solvent flow-rate, cartridges reusability, interference of plastic cartridges. For all the anabolics investigated the recoveries were greater than 83.6%.     

Study of the Capabilities of the ALICE inner tracking system stand-alone for HBT analysis

Results are shown from a Monte Carlo simulation study of the capabilities of the Inner Tracking System of the ALICE experiment, used in standalone mode, for HBT analysis of Pb?Pb collisions at LHC energies (5.5 ATeV). Different values of the coherence factor and the Gaussian source radius have been studied. For this purpose, a specific ITS stand-alone tracking algorithm, based on the Denby-Peterson neural algorithm, has been developed.     

A highly specific polyclonal antiserum to the environmental contaminant 1,1,1-trichloro-2,2-bis-(4-chlorophenyl)-ethane (p,p′-DDT)

A very selective polyclonal antiserum against 1,1,1-trichloro-2,2-bis-(4-chlorophenyl)-ethane (p,p′-DDT) was obtained by a careful choice of the haptenic structure (2,2-bis(4-chlorophenyl)-ethanol hemisuccinate). This hapten was conjugated to BSA to prepare the immunogen. The effects of different types of solid phases on the equilibrium reaction between the hapten on solid phase and the polyclonal antiserum were evaluated to obtain a fine tuning of the antiserum performances in terms of specificity for p,p′-DDT and sensitivity to low levels of this pesticide. The calibration curves obtained show that it is possible to set up a sensitive assay for p,p′-DDT, employing a p,p′-dichlorodiphenylacetic acid-based solid phase, with a detection limit of 0.12 ng/mL and a working range of about 0.21–40 ng/mL. Selectivity towards several p,p′-DDT-related substances was good (o,p-DDT 17%, p,p′-DDD 1.2% o,p-DDD 6.3%, p,p′-DDE 6.7%).