A parallel acquisition charged particle energy analyser using a magnetic field

A new form of charged particle energy analyser is proposed. It is broadly based on the 180° magnetic spectrograph, but is intended to detect charged particles moving out of the dispersion plane with a helical motion. The analyser has the capability to acquire charged particle energy spectra over a large energy range, similar to those acquired in Auger electron spectroscopy, ca. 2500 eV and large angular range, up to 90°, in parallel. These conditions are more favourable for surface analysis by electron spectroscopy at high vacuum, where for example an electron energy resolution of 0.2% to 0.5% is typical. Expressions showing how the landing positions of the charged particles on the detector vary as a function of energy and polar take off angle are determined as well as the conditions for optimum energy resolution at a range of polar take off angles. The equations reveal that in general, the device obtains the highest resolution at angles of revolution greater than 180°. The design is simple and could be easily put into practice using available material and technologies and be used to analyse the energies of electrons emitted from a sample placed in a scanning electron microscope. It can be made to function with a primary electron beam of any desired energy and could fit in to the small space between the sample and the end of an electron column. However, the device is difficult to retrofit into existing SEMs and ideally an SEM column needs to be designed to work in association with the analyser. The direction of the magnetic field of the analyser is coincident with the axis of the electron gun so that the primary beam is little influenced by the magnetic field and symmetry can be maintained in the primary beam electron column. Because the device is intended to acquire electron spectra in parallel, any movement of the primary beam on the sample because of a ramping field in the analyser is avoided. The field of view and the effect of the analyser upon the operation of the SEM are discussed. Spectra including elastic and Auger peaks reveal an energy resolution of ~4 eV at 900‐eV electron energy. Copyright © 2016 John Wiley & Sons, Ltd.     

Effect of atomic oxygen irradiation on the structural and tribological characteristics of polytetrafluoroethylene and its composites

Based on the ground‐based simulation facility, the effects of atomic oxygen (AO) irradiation on the structural and tribological properties of pure polytetrafluoroethylene (PTFE) and carbon fiber and MoS₂‐filled PTFE composites were studied by scanning electron microscopy, X‐ray photoelectron spectroscopy, and a ball‐on‐disc tribometer. The results shown that AO irradiation had significant effects on the structural and tribological properties of pure PTFE, in which the surface morphologies, mass loss, friction coefficient, and wear rate had been changed greatly after AO irradiation. However, it was noticeable that the addition of carbon fiber and MoS₂ filler to PTFE could improve the AO resist capacity and tribological properties of PTFE composites significantly. Copyright © 2016 John Wiley & Sons, Ltd.     

Probing the interfacial interaction between monolayer molybdenum disulfide and Au nanoclusters

Coupling of plasmonic metal nanostructures on two‐dimensional materials represents one promising approach to improve their optoelectronic device performance. In this article, we systematically investigated the interfacial interactions between Au nanoclusters and monolayer molybdenum disulfide (MoS₂) and the effect of Au decoration on the electrical transport and optical properties of MoS₂, through the combination of in situ MoS₂ field‐effect transistor device evaluation and in situ ultraviolet photoelectron spectroscopy and X‐ray photoelectron spectroscopy measurements. The in situ X‐ray photoelectron spectroscopy/ultraviolet photoelectron spectroscopy experiments revealed a weak interfacial coupling between Au nanoclusters and monolayer MoS₂. The absence of strong charge transfer between Au nanoclusters and MoS₂ was further confirmed by the photoluminescence and Raman measurements. It was also found that the electron charge‐carrier concentration in monolayer MoS₂ weakly depended on the coverage of Au nanoclusters. Copyright © 2017 John Wiley & Sons, Ltd.     

Synthesis of spiroindene-1,3-dione isothiazolines via a cascade michael/1,3-dipolar cycloaddition reaction of 1,3,4-oxathiazol-2-one and 2-arylidene-1,3-indandiones

The reaction of 1,3,4-oxathiazol-2-one derivative with 2-arylidene-1,3-indandione to furnish novel spiroindene-1,3-dione isothiazoline derivatives by Michael/1,3-dipolar [3+2]-cycloaddition reaction was investigated. The key 1,3-dipolar cycloaddition reaction step was examined in toluene solvent at reflux temperature to obtain mixture of two regioisomers (6a and 6b – 14a and 14b) and single isomers (15–20). The scope of this new reaction was demonstrated with many examples with high reactivity and yields.     

Synthesis of a secretoglobin 3A2 type C (98–139) fragment by Dawson’s native chemical ligation

A secretoglobin 3A2 type C (98–139) peptide was synthesized by native chemical ligation between ¹¹⁵Ile and ¹¹⁶Cys residues using Dawson’s linker. The peptide-N-acyl-benzimidazolinone-glycine amide, a C-terminal thioesters precursor, was provided from 3-amino-4-(methylamino)benzoic acid. In addition, an N-terminal cysteine fragment, the (116–139) peptide, was prepared by ordinary Fmoc-solid phase peptide synthesis. Native chemical ligation of the (98–115) fragment with the Dawson’s linker and the (116–139) peptide smoothly proceeded to give SCGB3A2 type C (98–139) peptide.     

Amphoteric 2-(sulfonylamino)benzaldehydes,secondary amines and isocyanides in the multicomponent synthesis of elusive N-alkyl-2,3-diaminoindoles

A novel interrupted Ugi reaction between ortho-sulfonylaminated aryl aldehydes, secondary amines, and isocyanides affords in good to high yields N-alkyl-2,3-diaminoindoles, providing access to a so far unexplored area of the indole chemical space. With only one single chemical operation, this novel reaction affords a broad gamma of substituted 2,3-diaminoindoles with five points of diversity. The success of this novel multicomponent transformation lies in presence of the amphoteric sulfonylamino group, which sequentially acts as a Brønsted acids and as a nucleophile the lack of need for additional catalysts and the high atom economy, with the loss of only one molecule of water, renders this approach a very effective one.     

A rapid and highly efficient Michael addition of methoxybenzenes and indoles to α,β-unsaturated ketones using BF3·OEt2 as a catalyst

An efficient and general protocol is described for the Michael addition of α,β-unsaturated ketones with electron-rich arenes/indoles to give alkylated arenes/indoles under mild reaction condition at room temperature. Shorter reaction time, convenient and good isolated yields are the significant features of this protocol. Moreover, the procedure is environmentally benign in nature and applicable to variety of arenes/indoles as well as α,β-unsaturated ketones.     

Anti-inflammatory chromone alkaloids and glycoside from Dysoxylum binectariferum

Herein we report isolation of a new chromone alkaloid chrotacumine K (12) from fruits and a chromone glycoside schumaniofioside A (13) from leaves of Dysoxylum binectariferum Hook f. Schumaniofioside A is reported for the first time from Meliaceae family. Other known alkaloids isolated include rohitukine (1) and chrotacumine E (6). The structure of new alkaloid 12 was elucidated on the basis of extensive 1D and 2D NMR analysis, synthesis and chemical hydrolysis. Chemically, chrotacumine K (12) is a 3′-O-acetyl rohitukine which on chemical or enzymatic hydrolysis produces rohitukine. The new alkaloid 12 is also present in seeds and stem-barks of this plant. The glycoside schumaniofioside A (13) is present only in leaves, and in abundance (～1% w/w of dried leaves). The isolated compounds and extracts were evaluated for in vitro effect on the proinflammatory cytokines (TNF-α and IL-6) in human monocytic THP-1 cells. The alkaloid 12 displayed potent inhibition (57%) of TNF-α at 0.3 µM, and was non-toxic to THP-1 cells up to 40 µM, indicating its excellent therapeutic window. Furthermore, a nitrobenzoyl ester analog 15e showed better inhibition of IL-6 than parent natural product chrotacumine K.     

New,simple, and efficient method for the synthesis of N-substituted 4-trifluoromethyl-5-(alkan-1-ol)-pyridin-2(1H)-imines

A new, simple, and efficient method for the synthesis a novel series of 1-substituted 4-(trifluoromethyl)-5-(alkan-1-ol)-pyridin-2(1H)-imines from the reaction of 3-(5,6-dihydro-4H-pyran-3-yl)-4,4,4-trifluorobut-2-enenitrile and 3-(4,5-dihydrofuran-3-yl)-4,4,4-trifluorobut-2-enenitrile with primary amines – is described. The products were obtained in 29–82% yield.     

Cobalt-catalyzed regioselective [3+2] annulation of ortho-formyl and acetyl substituted phenylboronic acids with alkynes

Treatment of alkynes with ortho-formyl and acetyl phenylboronic acids in the presence of a cobalt catalyst resulted in the formation of 2,3-disubstituted indenols in good yields. When aryl silyl alkynes were used, 2-aryl-3-silyl indenols were obtained regioselectively in good yields.