Mild and direct conversion of esters to morpholine amides using diisobutyl(morpholino)aluminum: application to efficient one-pot synthesis of ketones and aldehydes from esters

Morpholine amide intermediates, which are easily prepared by aminolysis of various esters with diisobutyl(morpholino)aluminum, react with organolithium and reducing agents (DIBALH or LDBMA) without isolation of the aminolysis intermediates to give ketones in 83–95% yields and aldehydes quantitatively.     

Indexing Non-merohedrally Twinned Crystals by Bruker'sAPEX2 and Agilent's CrysAlis~(PRO), an Example of a Crystal Structure That Can Be Refined through Either the PLATONRoute or the ‘HKLF 5' Route,and, Simultaneous Data Collection of Two Crystals in a Tw

The first part of this report describes the data reduction of non-merohedrally twinned crystals measured on Bruker and Agilent area-detector diffractometers. The image frames of methyl-2-aminopyrazine-3-carboxylate were processed with APEX2 to furnish a set of overlapping diffraction indices that were used for solution and refinement. CrysAlisPRO was used for processing the frames of bis(diethyldicarbamato)nickel, which exists in monoclinic and tetragonal polymorphs, and in untwinned and twinned forms. In the second part, the crystal structure of [(3-formyl-4- hydroxyphenyl)methyl]triphenylphosphanium chloride was refined through the ‘HKLF 5'(based on a combined set of diffraction indices) and PLATON(based on one set of diffraction indices) routes to give identical outcomes because the amount of overlap of the twin domains is small. For the third part, in a proof-of-concept investigation, the diffraction pattern of untwinned and twinned 4-{(E)-(4-aminophenyl)diazenyl]phenylamine was recorded simultaneously in one run; the three domains could be indexed and the crystal structure satisfactorily refined. The refinement was identical to those derived from independent measurements; the crystal structure features two independent centrosymmetric molecules, one of which is ordered and the other whole-molecule-disordered. This two-in-one run opens up the possibility that two or more crystals having different atomic compositions can be measured simultaneously if their reciprocal lattices do not overlap significantly.     

Propagation of mode shape errors in structural identification

It is of interest to the modal testing and health monitoring community to quantify how an error in any identified mode shape propagates to the identified flexibility matrix. Here this problem is investigated in a probabilistic framework. The approach followed involves deriving analytical expressions to track how errors, due to random deviations between identified and “true” mode shapes, propagate to the Modal Assurance Criterion (MAC) and the Coordinate Modal Assurance Criterion (COMAC) values as well as the estimated flexibility matrix. The comparison of the expected values and variances of these errors identifies the inconsistency between the magnitude of errors in the MAC and COMAC values and the identified flexibility matrix. The analytical results are further validated via Monte Carlo simulations. Finally, two mode shape comparison criteria, termed as the Flexibility Proportional Modal Assurance Criterion (FPMAC) and the Flexibility Proportional Coordinate Modal Assurance Criterion (FPCOMAC), are proposed. These new criteria aim to mimic the expected error in the predicted flexibility matrix in a direct comparison of the identified and “true” mode shapes, and hence they can be used to complement MAC and COMAC in interpreting the analysis results.     

Synthesis and characterization of thieno[3,2‐b]thiophene‐isoindigo‐based copolymers as electron donor and hole transport materials for bulk‐heterojunction polymer solar cells

A novel class of thieno[3,2‐b]thiophene (TT) and isoindigo based copolymers were synthesized and evaluated as electron donor and hole transport materials in bulk‐heterojunction polymer solar cells (BHJ PSCs). These π‐conjugated donor‐acceptor polymers were derived from fused TT and isoindigo structures bridged by thiophene units. The band‐gaps and the highest occupied molecular orbital (HOMO) levels of the polymers were tuned using different conjugating lengths of thiophene units on the main chains, providing band‐gaps from 1.55 to 1.91 eV and HOMO levels from ?5.34 to ?5.71 eV, respectively. The corresponding lowest unoccupied molecular orbital (LUMO) levels were appropriately adjusted with the isoindigo units. Conventional BHJ PSCs (ITO/PEDOT:PSS/active layer/interlayer/Al) with an active layer composed of the polymer and PC₇₁BM were fabricated for evaluation. Power conversion efficiency from a low of 1.25% to a high of 4.69% were achieved with the best performing device provided by the D?π?A polymer with a relatively board absorption spectrum, high absorption coefficient, and more uniform blend morphology. These results demonstrate the potential of this class of thieno[3,2‐b]thiophene‐isoindigo‐based polymers as efficient electron donor and hole transport polymers for BHJ PSCs. © 2012 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2013     

Poly[2,7‐(9,9‐dihexylfluorene)‐alt‐pyridine] with donor‐acceptor architectures: A new series of blue‐light‐emitting alternating copolymers

A novel series of well‐defined alternating poly[2,7‐(9,9‐dihexylfluorenyl)‐alt‐pyridinyl] (PDHFP) with donor‐acceptor repeat units were synthesized using palladium (0)‐catalyzed Suzuki cross‐coupling reactions in good to high yields. In this series of alternating polymers, 2, 7‐(9,9‐dihexylfluorenyl) was used as the light emitting unit, and the electron deficient pyridinyl unit was employed to provide improved electron transportation. These polymers were characterized by ¹H‐NMR and ¹³C‐NMR, gel permeation chromatography (GPC), thermal analyses, and UV‐vis and fluorescence spectroscopy. The glass transition temperature of copolymers in nitrogen ranged from 110 to 148 °C, and the copolymers showed high thermal stabilities with high decomposition temperatures in the range of 350 to 390 °C in air. The difference in linkage position of pyridinyl unit in the polymer backbone has significant effects on the electronic and optical properties of polymers in solution and in film phases. Meta‐linkage (3,5‐ and 2,6‐linkage) of pyridinyl units in the polymer backbone is more favorable to polymer for pure blue emission and prevention of aggregation of polymer chain than para‐linkage (2,5‐linkage) of the pyridinyl units. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 4792–4801, 2004     

Energy harvesting using multilayer structure based on 0.71Pb(Mg1/3Nb2/3)O3–0.29PbTiO3 single crystal

In this paper we fabricated the multilayer structure used as the resonance-based vibration energy-harvesting device based on 0.71Pb(Mg_1/3Nb_2/3)O₃–0.29PbTiO₃ single crystal. The performances of the device including the output voltage and power were studied systematically. Under a cyclic force of 4 N (peak value), a high output power of 4.94 mW and a corresponding peak voltage of 3.14 V were measured at 1.4 kHz with a matching load resistance of 1.0 kΩ. The results demonstrate the potential of the device in energy-harvesting applied to low-power portable electronics and wireless sensors.