Calixarenes as Polyhapto-aromatic Ligands: Alkali Metal Ions and Sulfonated Calixarenes

Crystal structure determinations for the hexarubidium and octacesium derivatives of calix[6]arene hexasulfonic acid, as well as of a new solvate of the pentasodium derivative of calix[4]arene tetrasulfonic acid, and comparison with structural data from the literature for alkali metal complexes of sulfonated calixarenes, have provided further evidence for the importance of interactions with aromatic ~ -electrons for the heavier alkali metal cations. There is evidence as well that this interaction can be enhanced by extended ionization of the sulfonated calixarene.     

Octahedral CuII and NiII complexes manifesting with N′-[1-(pyridin-2-yl)ethylidene] acetohydrazide: Structural outlooks and spectral characteristics

A tridentate hydrazone precursor, N′-[1-(pyridin-2-yl)ethylidene]acetohydrazide (L) (1:1 refluxed product of acetichydrazide and 2-acetylpyridine), produced two octahedral Cu^II and Ni^II derivatives, [CuL₂]·NO₃ (1) and [NiL₂]·ClO₄·H₂O (2). Both are subjected to X-ray diffraction system, and structural investigation shows that the central metal atom (Cu^II or Ni^II) adopts a distorted octahedral geometry with N₄O₂ donor sets by coordination of a pair of independent hydrazone precursors. Besides X-ray study, IR and UV-vis spectra, thermal analysis and room temperature magnetic moments are utilized for establishing significant characteristics of both complexes. It is apparent that the M-N_pyridine bonds are slightly longer than the M-N_imino bonds, Cu1-N1 and Cu1-N4 [2.300(2) and 2.038(2) ?] for 1 and Ni1-N1 and Ni1-N4 [2.075(2) and 2.084(1) ?] for 2, Cu1-N2 and Cu1-N5 [2.062(1) and 1.932(1) ?] for 1 and Ni1-N2 and Ni1-N5 [2.008(2) and 1.975(2) ?] for 2, respectively. As per our observation, the effective magnetic moment value (μ_eff) is found to be 1.77 B.M. for 1 and 3.06 BM for 2, respectively.     

At-line bioprocess monitoring by immunoassay with rotationally controlled serial siphoning and integrated supercritical angle fluorescence optics

In this paper we report a centrifugal microfluidic “lab-on-a-disc” system for at-line monitoring of human immunoglobulin G (hIgG) in a typical bioprocess environment. The novelty of this device is the combination of a heterogeneous sandwich immunoassay on a serial siphon-enabled microfluidic disc with automated sequential reagent delivery and surface-confined supercritical angle fluorescence (SAF)-based detection. The device, which is compact, easy-to-use and inexpensive, enables rapid detection of hIgG from a bioprocess sample. This was achieved with, an injection moulded SAF lens that was functionalized with aminopropyltriethoxysilane (APTES) using plasma enhanced chemical vapour deposition (PECVD) for the immobilization of protein A, and a hybrid integration with a microfluidic disc substrate. Advanced flow control, including the time-sequenced release of on-board liquid reagents, was implemented by serial siphoning with ancillary capillary stops. The concentration of surfactant in each assay reagent was optimized to ensure proper functioning of the siphon-based flow control. The entire automated microfluidic assay process is completed in less than 30 min. The developed prototype system was used to accurately measure industrial bioprocess samples that contained 10 mg mL⁻¹ of hIgG.     

Regioselective A-Ring Chlorination of Benzodiazepine Analogues Using tert-Butyl Hypochlorite

Treatment of 2-phenyl-2,3-dihydro-1,4-benzodiazepin-5(4H)-one and a series of 1,4-benzoxazepinone analogues with tert-butyl hypochlorite affords products shown, by NMR and MS spectroscopy, to be chlorinated exclusively in the A-ring at positions 7 and/or 9.     

An Improved Large Scale Synthesis of 2-Amino-4-chloropyridine and Its Use for the Convenient Preparation of Various Polychlorinated 2-Aminopyridines

An efficient large scale synthesis of 2-amino-4-chloropyridine (3) has been achieved through a modification of existing literature procedures. Compound 3 was used to prepare the previously unreported 2-amino-4,5-dichloropyridine (4). The known 2-amino-3,4-dichloropyridine (5) and 2-amino-3,4,5-trichloropyridine (6) were prepared from 3 by new routes and in higher yields than previously reported.     

Polarizing-alignment layers for twisted nematic cells

We describe polarizing films formed from the lyotropic liquid crystalline phases of dyes dissolved in water. The dye polarizers possess a high dichroic ratio close to that of conventional polarizers. In addition, the dried dye films provide a uniform homogeneous orientation for thermotropic nematic materials. Therefore, thin dye films can simultaneously serve as internal polarizers and as alignment agents. These properties make them especially suitable for twisted nematic devices based on low cost birefringent plastic substrates.