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11.
Morpholine amides are cheap and safe alternative to Weinreb amides as acylating agents of organometallic species. Herein, the in-situ lithiation/borylation of 18 ortho- meta- and para-substituted morpholine benzamides has been investigated. 10 of the 18 substrates provided the desired boronic esters as the major isomer (>90% regioselectivity) in crude isolated yields ranging from 68 to 93%. The synthetic usability of such building blocks was subsequently illustrated via the synthesis of a kinase inhibitor. 相似文献
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We employ a variables-in-common method for constructing multivariate Tweedie distributions, based on linear combinations of independent univariate Tweedie variables. The method lies on the convolution and scaling properties of the Tweedie laws, using the cumulant generating function for characterization of the distributions and correlation structure. The routine allows the equivalence between independence and zero correlation and gives a parametrization through given values of the mean vector and dispersion matrix, similarly to the Gaussian vector. Our approach leads to a matrix representation of multivariate Tweedie models, which permits the simulations of many known distributions, including Gaussian, Poisson, non-central gamma, gamma, and inverse Gaussian, both positively or negatively correlated. 相似文献
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Mark D. Noirot Elizabeth G. Bent Arlan D. Norman 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1-4):177-180
Abstract Reaction of the 1,3,2,4-diazadiphosphetidine, trans-[C6H5N(H)P(S)NC6H5]2 with LiR (R = Me, n-Bu) followed by treatment of the resulting dianions with Me3SiCl and Me3GeBr produced trans-[C6H5N(R)P(S)NC6H5]2(R = Me3Si, 2; Me3Ge, 3). Substitution occurs without cis-trans isomerization or significant cleavage of the 1,3,2,4-diazadiphosphetidine ring. 2 and 3 have been characterized by spectral (1H and 31P NMR, IR, and MS) and elemental analytical data. Analogous reactions involving Me3SnCl yield mixtures containing [C6H5N(SnMe3)P(S)NC6H5]2 which could not be isolated or completely characterized. 相似文献
16.
Ida‐Marie Hyvik Branislav Jansik Kasper Kristensen Poul Jrgensen 《Journal of computational chemistry》2013,34(15):1311-1320
Using the three‐level energy optimization procedure combined with a refined version of the least‐change strategy for the orbitals—where an explicit localization is performed at the valence basis level—it is shown how to more efficiently determine a set of local Hartree–Fock orbitals. Further, a core–valence separation of the least‐change occupied orbital space is introduced. Numerical results comparing valence basis localized orbitals and canonical molecular orbitals as starting guesses for the full basis localization are presented. The results show that the localization of the occupied orbitals may be performed at a small computational cost if valence basis localized orbitals are used as a starting guess. For the unoccupied space, about half the number of iterations are required if valence localized orbitals are used as a starting guess compared to a canonical set of unoccupied Hartree–Fock orbitals. Different local minima may be obtained when different starting guesses are used. However, the different minima all correspond to orbitals with approximately the same locality. © 2013 Wiley Periodicals, Inc. 相似文献
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Maj-Britt Schmidt Andersen Mette Kristensen Claudine Manach Estelle Pujos-Guillot Sanne Kellebjerg Poulsen Thomas Meinert Larsen Arne Astrup Lars Dragsted 《Analytical and bioanalytical chemistry》2014,406(7):1829-1844
While metabolomics is increasingly used to investigate the food metabolome and identify new markers of food exposure, limited attention has been given to the validation of such markers. The main objectives of the present study were to (1) discover potential food exposure markers (PEMs) for a range of plant foods in a study setting with a mixed dietary background and (2) validate PEMs found in a previous meal study. Three-day weighed dietary records and 24-h urine samples were collected three times during a 6-month parallel intervention study from 107 subjects randomized to two distinct dietary patterns. An untargeted UPLC-qTOF-MS metabolomics analysis was performed on the urine samples, and all features detected underwent strict data analyses, including an iterative paired t test and sensitivity and specificity analyses for foods. A total of 22 unique PEMs were identified that covered 7 out of 40 investigated food groups (strawberry, cabbages, beetroot, walnut, citrus, green beans and chocolate). The PEMs reflected foods with a distinct composition rather than foods eaten more frequently or in larger amounts. We found that 23 % of the PEMs found in a previous meal study were also valid in the present intervention study. The study demonstrates that it is possible to discover and validate PEMs for several foods and food classes in an intervention study with a mixed dietary background, despite the large variability in such a dataset. Final validation of PEMs for intake of foods should be performed by quantitative analysis. Figure
Examples of two urinary exposure markers for cabbage (left) and beetroot (right) found in the study from an untargeted LC‐MS metabolomics analysis of urine samples and self‐reported food intake data 相似文献
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Jacobsen AM Halling-Sørensen B Ingerslev F Hansen SH 《Journal of chromatography. A》2004,1038(1-2):157-170
The veterinary antibacterial agents chlortetracycline (CTC), oxytetracycline (OTC), sulfadiazine (SDZ), erythromycin (ERY) and tylosin (TYL A, B, C and D) were extracted from soil using pressurized liquid extraction (PLE). Citric acid (pH 4.7) and methanol was used as extraction buffer, followed by tandem-solid-phase extraction (SPE) clean-up (SAX + HLB) for all compounds. For quantification two slightly different methods were employed using LC-MS-MS with MRM detection. The soil extraction method was validated using a loamy sand soil and a sandy soil, representing two typical Danish agricultural soils. Recoveries were 50-80% for the tetracyclines (CTC and OTC) and sulfadiazine (SDZ) and 60-100% for the macrolides (TYL and ERY). Limits of detection for the soil extraction method (LOD(soil)) were 0.6-5.6 microg kg(-1) soil for CTC and OTC, 0.9-2.9 microg kg(-1) soil for SDZ and 2.4-5.5 microg kg(-1) soil for TYL A and ERY. Furthermore, the method was applied to field samples taken from two agricultural fields fertilised with liquid manure containing CTC and TYL A. These results showed a decline in the content of antibacterial agents throughout the sampling period of 155 days from 10 to 15 microg CTC kg(-1) soil and 20-55 microg TYL A kg(-1) soil to below or near the LOD(soil) listed above. Finally, the method was applied to barley grains harvested from the fields. None of the antibacterial agents were measured in grain samples, but recoveries for spiked grain samples were similar to soil recoveries. 相似文献
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N. T. Zinner G. M. Bruun 《The European Physical Journal D - Atomic, Molecular, Optical and Plasma Physics》2011,65(1-2):133-139
A layered system of two-dimensional planes containing fermionic polar molecules can potentially realize a number of exotic quantum many-body states. Among the predictions, are density-wave instabilities driven by the anisotropic part of the dipole-dipole interaction in a single layer. However, in typical multilayer setups it is reasonable to expect that the onset and properties of a density-wave are modified by adjacent layers. Here we show that this is indeed the case. For multiple layers the critical strength for the density-wave instability decreases with the number of layers. The effect depends on density and is more pronounced in the low density regime. The lowest solution of the instability corresponds to the density waves in the different layers being in-phase, whereas higher solutions have one or several adjacent layers that are out of phase. The parameter regime needed to explore this instability is within reach of current experiments. 相似文献