A Practical and Enantiospecific Synthesis of (−)‐(R)‐ and (+)‐(S)‐Piperidin‐3‐ols

A highly enantiospecific, azide‐free synthesis of (?)‐(R)‐ and (+)‐(S)‐piperidin‐3‐ol in excellent yield was developed. The key step of the synthesis involves the enantiospecific ring openings of enantiomerically pure (R)‐ and (S)‐2‐(oxiran‐2‐ylmethyl)‐1H‐isoindole‐1,3(2H)‐diones with the diethyl malonate anion and subsequent decarboxylation.     

A phenolic glycoside from artemisia sacrorum

A phenolic glycoside has been isolated from Artemisia sacrorum grown in the Northeast of China. This compound is identified to be 4-O-β-D-glucopyranosyl-2-O-methylphloroacetophenone by means of nmr spectroscopy and synthesis.     

Synthesis of Quinoline Analogs: Search for Antimalarial Agents

Summary. Novel synthesis routes for the promising antimalarial agents 4(3-hydroxypyrrolidin-1-yl) and 4(3-hydroxypiperidine-1-yl)-2,8-bis(trifluoromethyl)quinoline have been developed.     

PHYCOERYTHROCYANINS FROM Westiellopsis prolifica AND Nostoc rivulare: CHARACTERIZATION OF THE PHYCOVIOLOBILIN CHROMOPHORE IN BOTH STATES*

Abstract— Phycoerythrocyanin or fractions enriched in it have been isolated from the filamentous cyanobacteria, Westiellopsis prolifica ARM 365 and Nostoc rivulare ARM 212. Both show the photoreversible photochromism (difference maxima at 503 and 570 nm) characteristic of this pigment, which is related to the phycoviolobilin chromophore on the α-subunit. Native phycoerythrocyanin and its β-subunit show little if any reversible photochemistry in the 600–620 nm region, where the phycocyanobilin chromophores absorb maximally. Instead the phycocyanobilin chromophores are bleached irreversibly. At the same time, the data show that reversible photochemistry is a useful analytical tool to detect phycoerythrocyanin in cyanobacterial extracts. Fluorescence measurements indicate that: (i) the 510 nm absorbing isomer of the violobilin chromophore has only little fluorescence; and (ii) the energy transfer from the violobilin chromophores to the cyanin chromophores is efficient only in the 570 nm form.     

Iodine-mediated facile dehydrogenation of dihydropyridazin-3(2H)one

A new protocol for the dehydrogenation of dihydropyridazin-3(2H)-one has been carried out by catalytic amount of iodine in dimethyl sulphoxide in good yield with easy workup.     

Conformational analysis of c3′-c8 connected biflavones

Two biflavones isolated from Taxus cuspidata were identified with ginkgetin (1) and sciadopitysin (2) which belong to C3′-C8 connected biflavones. The conformation of 2 in the solid state was determined by X-ray analysis and the conformations of 1 and 2 in the liquid state were discussed using nmr techniques. Complete assignments of ¹H and ¹³C nmr spectra about 1 were made on the basis of COSY, HMQC, HMBC and nOe experiments.     

Surface Molding of Microscale Hydrogels with Microactuation Functionality

This work describes the fabrication of numerous hydrogel microstructures (μ‐gels) via a process called “surface molding.” Chemically patterned elastomeric‐assembly substrates were used to organize and manipulate the geometry of liquid prepolymer microdroplets, which, following photo‐initiated crosslinking, maintained the desired morphology. By adjusting the state of strain during the crosslinking process, a continua of structures could be created using one pattern. These arrays of μ‐gels have stimuli‐responsive properties that are directly applicable to actuation where the basis shape and array geometry of the μ‐gels can be used to rationally generate microactuators with programmed motions. As a method, “surface molding,” represents a powerful addition to the soft‐lithographic toolset that can be readily applied to the simultaneous synthesis of large numbers of geometrically and functionally distinct polymeric microstructures.     

Binding of the general anesthetics chloroform and 2,2,2-trichloroethanol to the hydrophobic core of a four-alpha-helix bundle proteins

The structural features of general anesthetic binding sites on proteins are being examined using a defined model system consisting of a four-alpha-helix bundle scaffold with a hydrophobic core. Previous work suggested that halothane binding to the four-alpha-helix bundle was improved by (1) introducing a cavity into the hydrophobic core and (2) substituting a methionine side-chain in place of an alpha-helical heptad e position leucine. In this study, the ability of the general anesthetics chloroform and 2,2,2-trichloroethanol to bind to the hydrophobic core of the four-alpha-helix bundle (Aalpha2-L38M)2 is explored. The halogenated alkane chloroform binds with a dissociation constant (Kd) = 1.4 +/- 0.2 mM, whereas 2,2,2-trichloroethanol binds with a Kd = 19.5 +/- 1.2 mM. The affinity of both general anesthetics for the hydrophobic core of the four-alpha-helix bundle approximates their whole animal effective concentration in 50% of test subjects' (EC50) values, as shown previously for halothane. Tryptophan phosphorescence decay rates at 77 K are accelerated by a factor of 4.5 by both bound halothane and chloroform, indicating that the heavy-atom effect is responsible for a portion of the observed fluorescence quenching. Because heavy-atom effects are operative only at short distances, the findings indicate that these general anesthetics are binding in the vicinity of the indole rings of W15 in the hydrophobic core of the four-alpha-helix bundle scaffold. The results indicate that chloroform, halothane and 2,2,2-trichloroethanol may occupy the same sites on protein targets.     

High-performance liquid chromatography column switching applied to the trace determination of herbicides in environmental and drinking water samples

A selective and sensitive coupled-column high-performance liquid chromatographic method is developed for the simultaneous determination of 5 phenylurea herbicides (monuron, linuron, isoproturon, monolinuron, and diuron) in environmental and drinking water samples. Sample clean-up is performed automatically by means of a column switching technique. Using 2 octadecyl silica columns connected via two programmable 6-port valves and ultraviolet detection at 244 nm, the aforementioned compounds can be determined at the low concentration levels required for pesticide residue analysis in water samples. A mobile phase consisting of a mixture of methanol-water (55:45, v/v) is pumped at 1 mL/min. For the 5 phenylureas, high recoveries ranging from 94.9 to 101.6%, good reproducibility with relative standard deviations lower than 5%, and wide linear ranges up to 20 micrograms/L are observed with determination limits of 0.05 microgram/L. The method is successfully applied to the screening of different environmental water samples such as surface, ground, rain, and drinking water.     

Determination of ofloxacin in tablets by room-temperature phosphorimetry on a poly(vinyl alcohol) solid substrate

An easy and sensitive method for the quantitative determination of ofloxacin (OFLX), a new fluoroquinolone antimicrobial agent, in a pharmaceutical formulation, tablet, was developed by using solid-substrate room-temperature phosphorimetry (RTP) on a poly(vinyl alcohol) substrate. The method did not require a dry gas flush during the measurement of phosphorescence. The influence of different conditions such as solution pH and concentrations of heavy atoms, used as the enhancer, were studied. The phosphorescence intensity of OFLX was enhanced using NaOH and KI as enhancers. A linear relationship between concentration and RTP intensity for each standard solution was obtained in the concentration range of 4-18000 ng/ml, and the determination limit was 4 ng/ml. The proposed method was applied to a determination of OFLX in a commercial tablet, and the results were compared with those of fluorescence and UV methods. It was proven that OFLX in a commercial tablet can be accurately measured by this method with a very small amount of sample solution.