β-Lactone as intermediate in the perkin reaction catalyzed by tertiary amines

The Perkin reaction catalyzed by tertiary amines is found to run not according to the aldol-type condensation mechanism but according to the mechanism in which the first stage is the formation and cycloaddition of ketene, yielding a β-lactone, which cleaves to the unsaturated acid.     

Ultrasonic inspection of batters for on-line process monitoring

A new method for on-line batter monitoring using ultrasound techniques is presented. Air or gas incorporation is done during the beating process which produces bubbles in the mixture. The density and the compressibility of the batter vary as a function of mixing time and are quality index of batter. Traditionally, a batter sample of a fixed volume is removed and weighted in order to determine its density. This is a time consuming process. Batters are air filled mixtures of high viscosity which do not support significant transmission of ultrasound. For this reason conventional ultrasonic density sensors for liquids are not suitable for this application. Therefore, a special transducer has been developed. The sensor was constructed using a piezoelectric ceramic at the fundamental frequency of 1 MHz. Instead of measuring density, in this work, changes in compressibility in batters are monitored by measuring the acoustic impedance of the batter. Main advantage of this novel approach is that changes in acoustic impedance are easier to detect than changes in density especially when air incorporation is in small quantities. Experimental results on different liquids and batters with different gas contents are presented and discussed.     

Eavesdropping on the "ping-pong" quantum communication protocol

Security of the "ping-pong" quantum communication protocol recently proposed by Bostr?m and Felbinger [Phys. Rev. Lett. 89, 187902 (2002)]] is analyzed in the case of considerable quantum channel losses. The eavesdropping scheme is presented, which reveals that the ping-pong protocol is not secure for transmission efficiencies lower than 60%. Our scheme induces 50% losses, which, however, can be hidden in the channel losses if one replaces the original lossy channel with a less lossy one. Finally, a possible improvement of the ping-pong protocol security is proposed.     

Determination of 61 organic pollutants in drinking water by solid phase extraction followed by liquid and gas chromatography coupled to tandem mass spectrometry: an analytical strategy for a routine laboratory

A method for determination of 61 organic pollutants (polycyclic aromatic hydrocarbons and organochlorine, organophosphorous and organonitrogen pesticides) is proposed. It is based on solid phase extraction (SPE) and subsequent analysis of the extract by liquid and gas chromatography coupled to tandem mass spectrometry. Method validation yielded to the following values: limits of quantification, from 0.005 to 0.020?µg?L^?1; trueness, 95% to 113% and reproducibility (as percent relative standard deviation), 2% to 15%. Additionally, the method performed well in various proficiency tests.     

A Convenient Stereoselective Synthesis of (1R,2S,3R,4S)-3-(Neopentyloxy)isoborneol

A convenient preparation of (1R,2S,3R,4S)-3-(neopentyloxy)isoborneol (= (1R,2S,3R,4S)-3-(2,2-dimethyl-propoxy)-1,7,7-trimethylbicyclo[2.2.1]heptan-2-ol; 1a ), a valuable chiral auxiliary, is described. The synthesis involves six steps starting from the readily available camphorquinone ( 5 ) and gives 1a in 48% overall yield. The key step is the chemoselective hydrolysis of the less hindered 1,3-dioxolane moiety in the camphorquinone di-acetal 4 .     

Determination of aminoglycoside residues in kidney and honey samples by hydrophilic interaction chromatography‐tandem mass spectrometry

Two methods based on liquid chromatography–tandem mass spectrometry were developed for the determination of ten aminoglycosides (streptomycin, dihydrostreptomycin, spectinomycin, apramycin, paromomycin, kanamycin A, gentamycin C1, gentamycin C2/C2a, gentamycin C1a, and neomycin B) in kidney samples from food‐producing animals and in honey samples. The methods involved extraction with an aqueous solution (for the kidney samples) or sample dissolution in water (for the honey samples), solid‐phase extraction with a weak cation exchange cartridge and injection of the eluate into a liquid chromatography–tandem mass spectrometry system. A zwitterionic hydrophilic interaction chromatography column was used for separation of aminoglycosides and a triple quadrupole mass analyzer was used for detection. The methods were validated according to Decision 2002/657/EC. The limits of quantitation ranged from 2 to 125 μg/kg in honey and 25 to 264 μg/kg in the kidney samples. Interday precision (RSD%) ranged from 6 to 26% in honey and 2 to 21% in kidney. Trueness, expressed as the percentage of error, ranged from 7 to 20% in honey and 1 to 11% in kidney.     

Modular bis(oxazoline) ligands for palladium catalyzed allylic alkylation: unprecedented conformational behaviour of a bis(oxazoline) palladium eta3-1,3-diphenylallyl complex

New families of enantiopure bis(oxazolines) with 4,5-trans (5 a-g) or 4,5-cis (6 c) stereochemistry at the individual rings have been prepared in high yield. Their eta(3)-allyl palladium complexes (8 a-g, 9 c and 10) have been used as catalytic precursors in allylic alkylation reactions with excellent enantioselectivities (up to 96 %) for the trans oxazoline derivatives, while Pd/6 c system was inactive. NMR studies on palladium eta(3)-1,3-diphenylallyl intermediates (11 a, c and e) showed the presence of syn/syn- and syn/anti-allyl isomers in solution; this resembles the first example of eta(3)-eta(1)-eta(3) isomerism in Pd allylic complexes containing bis(oxazolines) derived from malonic acid.