Continuous Krapcho Dealkoxycarbonylation in API Synthesis

A high pressure and high temperature continuous flow reactor has been used to intensify a Krapcho dealkoxycarbonylation reaction in the context of API synthesis. The reactor enables operation of the reaction above temperatures possible in batch and thus significantly increased conversion rates are achieved. Also a broader choice of solvents is possible by the use of the continuous process. Batch and continuous reaction are compared in terms of operation range and space-time-yield. Despite lower concentrations of the reactants in the continuous process, space-time-yield exceeds that of the batch process by more than an order of magnitude due to the higher reaction rates

Accuracy of low-dose computed tomography coronary angiography using prospective electrocardiogram-triggering: first clinical experience

AIMS: To evaluate the accuracy of low-dose computed tomography coronary angiography (CTCA) using prospective ECG-triggering for the assessment of coronary artery disease (CAD). METHODS AND RESULTS: A total of 30 patients (19 males, 11 females, mean age 58.8 +/- 9.9 years) underwent low-dose CTCA and invasive coronary angiography (CA) [median 2 days (0, 41)]. Before CT scanning, intravenous beta-blocker was administered in 18 of 30 patients as heart rate (HR) was >65 b.p.m., achieving a mean HR of 55.7 +/- 7.9 b.p.m. CAD was defined as coronary artery narrowing > or =50%, using CA as standard of reference. The estimated mean effective radiation dose was 2.1 +/- 0.7 mSv (range: 1.0-3.3), yielding 96.0% (383/399) of evaluable segments. On an intention-to-diagnose-base, all non-evaluative segments were included in the analysis. Vessels with a non-evaluative segment and no further finding were censored as false positive. Patient-based analysis revealed sensitivity, specificity, positive predictive value, and negative predictive value of 100, 83.3, 90.0, and 100%, respectively. The respective values per vessel were 100, 88.9, 85.7, and 100%, respectively. CONCLUSION: Prospective ECG-triggering allows low-dose CTCA and provides high diagnostic accuracy in the assessment of CAD in patients with stable sinus rhythm and a low heart rat

Feasibility of low-dose coronary CT angiography: first experience with prospective ECG-gating

AIMS: To determine the feasibility of prospective electrocardiogram (ECG)-gating to achieve low-dose computed tomography coronary angiography (CTCA). METHODS AND RESULTS: Forty-one consecutive patients with suspected (n = 35) or known coronary artery disease (n = 6) underwent 64-slice CTCA using prospective ECG-gating. Individual radiation dose exposure was estimated from the dose-length product. Two independent readers semi-quantitatively assessed the overall image quality on a five-point scale and measured vessel attenuation in each coronary segment. One patient was excluded for atrial fibrillation. Mean effective radiation dose was 2.1 +/- 0.6 mSv (range, 1.1-3.0 mSv). Image quality was inversely related to heart rate (HR) (57.3 +/- 6.2, range 39-66 b.p.m.; r = 0.58, P 63 b.p.m. (P < 0.001). CONCLUSION: This first experience documents the feasibility of prospective ECG-gating for CTCA with diagnostic image quality at a low radiation dose (1.1-3.0 mSv), favouring HR <63 b.p.

Feasibility of low-dose coronary CT angiography: first experience with prospective ECG-gating

AIMS: To determine the feasibility of prospective electrocardiogram (ECG)-gating to achieve low-dose computed tomography coronary angiography (CTCA). METHODS AND RESULTS: Forty-one consecutive patients with suspected (n = 35) or known coronary artery disease (n = 6) underwent 64-slice CTCA using prospective ECG-gating. Individual radiation dose exposure was estimated from the dose-length product. Two independent readers semi-quantitatively assessed the overall image quality on a five-point scale and measured vessel attenuation in each coronary segment. One patient was excluded for atrial fibrillation. Mean effective radiation dose was 2.1 +/- 0.6 mSv (range, 1.1-3.0 mSv). Image quality was inversely related to heart rate (HR) (57.3 +/- 6.2, range 39-66 b.p.m.; r = 0.58, P 63 b.p.m. (P < 0.001). CONCLUSION: This first experience documents the feasibility of prospective ECG-gating for CTCA with diagnostic image quality at a low radiation dose (1.1-3.0 mSv), favouring HR <63 b.p.

Linear magnetoresistance in commercial n-type silicon due to inhomogeneous doping

Free electron theory tells us that resistivity is independent of magnetic field. In fact, most observations match the semiclassical prediction of a magnetoresistance that is quadratic at low fields before saturating. However, a non-saturating linear magnetoresistance has been observed in exotic semiconductors such as silver chalcogenides, lightly-doped InSb, N-doped InAs, MnAs-GaAs composites, PrFeAsO, and epitaxial graphene. Here we report the observation of a large linear magnetoresistance in the ohmic regime in commonplace commercial n-type silicon wafer. It is well-described by a classical model of spatially fluctuating donor densities, and may be amplified by altering the aspect ratio of the sample to enhance current-jetting: increasing the width tenfold increased the magnetoresistance at 8 T from 445 % to 4707 % at 35 K. This physical picture may well offer insights into the large magnetoresistances recently observed in n-type and p-type Si in the non-ohmic regime.Comment: submitted to Nature Material

Nuclear myocardial perfusion imaging with a cadmium-zinc-telluride detector technique: optimized protocol for scan time reduction

We aimed at establishing the optimal scan time for nuclear myocardial perfusion imaging (MPI) on an ultrafast cardiac gamma-camera using a novel cadmium-zinc-telluride (CZT) solid-state detector technology. METHODS: Twenty patients (17 male; BMI range, 21.7-35.5 kg/m(2)) underwent 1-d (99m)Tc-tetrofosmin adenosine stress and rest MPI protocols, each with a 15-min acquisition on a standard dual-detector SPECT camera. All scans were immediately repeated on an ultrafast CZT camera over a 6-min acquisition time and reconstructed from list-mode raw data to obtain scan durations of 1 min, 2 min, etc., up to a maximum of 6 min. For each of the scan durations, the segmental tracer uptake value (percentage of maximum myocardial uptake) from the CZT camera was compared by intraclass correlation with standard SPECT camera data using a 20-segment model, and clinical agreement was assessed per coronary territory. Scan durations above which no further relevant improvement in uptake correlation was found were defined as minimal required scan times, for which Bland-Altman limits of agreement were calculated. RESULTS: Minimal required scan times were 3 min for low dose (r = 0.81; P < 0.001; Bland-Altman, -11.4% to 12.2%) and 2 min for high dose (r = 0.80; P < 0.001; Bland-Altman, -7.6% to 12.9%), yielding a clinical agreement of 95% and 97%, respectively. CONCLUSION: We have established the minimal scan time for a CZT solid-state detector system, which allows 1-d stress/rest MPI with a substantially reduced acquisition time resulting in excellent agreement with regard to uptake and clinical findings, compared with MPI from a standard dual-head SPECT gamma-camera

Metal-insulator Crossover Behavior at the Surface of NiS_2

We have performed a detailed high-resolution electron spectroscopic investigation of NiS$_2$ and related Se-substituted compounds NiS$_{2-x}$Se$_x$, which are known to be gapped insulators in the bulk at all temperatures. A large spectral weight at the Fermi energy of the room temperature spectrum, in conjunction with the extreme surface sensitivity of the experimental probe, however, suggests that the surface layer is metallic at 300 K. Interestingly, the evolution of the spectral function with decreasing temperature is characterized by a continuous depletion of the single-particle spectral weight at the Fermi energy and the development of a gap-like structure below a characteristic temperature, providing evidence for a metal-insulator crossover behavior at the surfaces of NiS$_2$ and of related compounds. These results provide a consistent description of the unusual transport properties observed in these systems.Comment: 12 pages, 3 figure

Scaling of the Conductivity with Temperature and Uniaxial Stress in Si:B at the Metal-Insulator Transition

Using uniaxial stress to tune Si:B through the metal-insulator transition we find the conductivity at low temperatures shows an excellent fit to scaling with temperature and stress on both sides of the transition. The scaling functions yield the conductivity in the metallic and insulating phases, and allow a reliable determination of the temperature dependence in the critical regions on both sides of the transition