The facile synthesis of benzothiazolylideneacetates and 1,4-benzothiazines through a highly controllable oxidation of benzothiazolylacetates

The synthesis of benzothiazolylideneacetates and 1,4-benzothiazine was found to be highly controllable via simple exchange of corresponding oxidants. It turned out that the treatment of benzothiazolylacetates with m-CPBA gave 1,4-benzothiazines via oxidative ring expansion process, and with DDQ gave benzothiazolylideneacetates via dehydrogenation, in good yield, respectively. The structures of both skeletons were confirmed by their X-ray diffractions. A previously reported method for the synthesis of benzothiazolylideneacetates was thus proved to be incorrect.     

Thermally-induced optical bistability with two holding beams

Thermally-induced optical bistability with two holding beams has been experimentally investigated in a metal-dielectric-metal interference mirror. Steady-state responses different from the usual S-shaped curve and with potential interest for composite logic operations are reported.     

AT-free图的配对控制集算法

本文给出了配对控制集在AT-free图的BFS-树上分布的结构性质．利用这些性质，我们给出了求解AT-free图类最小配对控制集的多项式时间算法．     

On the origin of anomalous soft photons in muon-proton interactions at high energy

We present arguments supporting the conjecture that anomalous prompt photons observed recently in muon-proton interactions by the European Muon Collaboration (EMC) at CERN are of the same dynamical origin as low mass lepton pairs produced in hadronic collisions. The EMC data are found to be in a qualitative agreement with the soft annihilation model. The conjecture implies that the rate of anomalous photon production depends quadratically on the rapidity density of secondary hadrons in the rapidity region of the photon. A study of this dependence is suggested as a crucial test of the conjecture.     

Generation of a novel monoclonal antibody against cortisol-[C-4]-bovine serum albumin conjugate: application to enzyme-linked immunosorbent assay for urinary and serum cortisol.

Measurement of cortisol levels in body fluids is important for monitoring pituitary gland and adrenal functions. To develop a specific and standardized enzyme-linked immunosorbent assay (ELISA), a novel monoclonal anti-cortisol antibody has been generated using a reasonably designed haptenic derivative. Spleen cells were prepared from the BALB/c or A/J mouse, which had repeatedly been immunized with a conjugate of 4-(2-carboxyethylthio)cortisol (CET) and bovine serum albumin, to be fused with P3/NS1/1-Ag4-1 myeloma cells. After four fusion experiments, one hybridoma clone secreting a practical antibody has been established. The resulting monoclonal antibody CS#38 (isotype gamma1, kappa) showed an affinity constant (K(a)) for cortisol of 1 x 10(9) M(-1) and provided a practical calibration curve (detection limit, 0.26 ng per assay) in a homologous ELISA system employing horseradish peroxidase-labeled CET as a labeled antigen. Cross-reactivities with related C-21 steroids were acceptably low: 11-deoxycortisol (4.3%), cortisone (4.0%), corticosterone (1.9%), progesterone (1.6%), 17alpha-hydroxyprogesterone (12%), 6beta-hydroxycortisol (8.4%), and tetrahydrocortisol (< 0.1%). Urinary and serum cortisol levels of healthy volunteers were determined by this method after methylene chloride extraction to be 39.0 +/- 17.0 microg/day (n = 7) and 80.8 +/- 38.9 ng/mL (n = 10), respectively, both of which are in the reference range.     

Photophysics and Photochemistry of z‐Chlorprothixene in Acetonitrile†

Chlorprothixene (CPTX, Taractan^®) is a low potency antipsychotic mainly used for the treatment of psychotic disorders (e.g. schizophrenia) and acute mania occurring as part of bipolar disorders. As in the case of other numerous drugs used in the treatment of psychiatric disorders, CPTX presents geometric isomerism. Therefore, in vitro irradiation induces a rapid Z/E isomerization, which can affect its pharmacokinetic properties. This photoisomerization is not dependent on the oxygen concentration. The Z/E quantum yields determined for zCPTX in acetonitrile are 0.22 and 0.21 in anaerobic and aerobic environments, respectively. In the presence of water, both isomers decompose to produce 2‐chlorothioxanthone (CTX) after prolonged irradiation. This process strongly depends on the water concentration and the irradiation time, i.e. it is autocatalyzed by the CTX through a triplet‐energy transfer mechanism. The protonation state of the terminal amino group, on the other hand, has no effect on the isomerization process, but inhibits the formation of CTX. These results indicate that the phototoxicity of zCPTX is somehow affected by the formation of CTX.     

The facile one-pot synthesis of N-imidoylbenzotriazoles via a Beckmann rearrangement of ketoximes

N-Imidoylbenzotriazoles 2a-m were obtained in good to excellent yields (up to 97%) by the reaction of ketoximes 1a-m with MsCl and subsequently with benzotriazole as a one-pot process in Toluene/CH₃CN at reflux temperature via a Beckmann rearrangement.     

A fused donor-acceptor system based on an extended tetrathiafulvalene and a ruthenium complex of dipyridoquinoxaline

An application of the Horner-Wadsworth-Emmons reaction carried out on a ruthenium compound as the electrophilic precursor is described for the synthesis of fused donor-acceptor system 1 based on an extended tetrathiafulvalene and a ruthenium complex of dipyridoquinoxaline units.     

An APCI LC‐MS/MS method for routine determination of capecitabine and its metabolites in human plasma

The anticancer drug capecitabine and its metabolites [including the active metabolite 5‐fluorouracil (5‐FU)] display high pharmacokinetic inter‐patient variability. Such variability, which may lead to treatment failure or toxicity, could need drug concentration measurement to individualize dosing regimen. However, usual assay methods are often long and fastidious. A simultaneous and cost‐effective method was thus developed for the determination of the concentrations of these compounds in human plasma. Compounds were extracted via a classic liquid–liquid extraction. Chromatographic analysis was performed on a C18 reverse phase column with detection by atmosphere pressure chemical ionization LC‐MS/MS. Our method allows a good chromatographic separation of the compounds and was fully validated following Food and Drug Administration (FDA) recommendations (good selectivity, no carry‐over, linearity of the calibration curves without weighting, deviations from nominal concentrations of standard samples lower than 15%, intra‐ and inter‐assay precision and accuracy lower than 15%). Recovery and stability were also acceptable following the FDA guidelines. A matrix effect impairing the determination of 5‐FU was avoided by using a stable isotopic derivative of 5‐FU as internal standard. Interestingly, this method allows detection of TetraHydroUridine, an inhibitor of ex vivo degradation of metabolites, which is essential for the stability, the adequate conditioning of blood samples and for good laboratory practice, essential in routine determination. This method seems usable to routinely determine concentrations of capecitabine and its metabolites in blood and may be helpful in further studies aiming at performing therapeutic drug monitoring. Copyright © 2010 John Wiley & Sons, Ltd.