Elimination of the 4-hydroxyl group of the alkaloids related to morphine—I

Sinomenine, an alkaloid of the Japanese plant Sinomenium acutum, was converted to the 4-phenylether by the Ullmann reaction in a good yield. The Clemmensen reduction of sinomenine-phenylether and of its derivatives gave (+)-3-methoxy-4-phenoxy-N-methyl-Δ^x-morphinan.

Hydrogenation and successive sodium-liquid ammonia reduction of (+)-3-methoxy-4-phenoxy-N-methyl-Δ^x-morphinan gave (+)-3-methoxy-N-methylmorphinan.     

Luminescence determination of benzoquinoline isomers in complex samples

The room-temperature phosphorescence (r.t.p.) and fluorescence spectra of benzoquinoline isomers are investigated. The isomers can be resolved into the linear or angular subgroups on the basis of their fluorescence and r.t.p. spectra by using conventional fixed excitation. Second-derivative and synchronous scanning techniques can be combined to improve the selectivity of the r.t.p. and fluorescence methods. These simple luminescence techniques were used to estimate three benzoquinoline isomers in a coal tar fraction. Direct analysis of this complex sample allowed acridine to be estimated and upper limits to be provided for benzo(h)quinoline and phenanthridine; the presence of three other isomers was not detected. Comparative studies with data obtained by high-performance liquid chromatography are reported.     

Reactivity and characterisation of various rank turkish bituminous coal chars

A set of seven bituminous coal chars has been characterised by IR spectroscopy (FTIR), thermogravimetry (TG) and elemental analysis. FTIR study provided suitable information to establish differences between coal samples according to their chemical compositions. The reactivity of these samples was also studied and correlated with the coal parameters of mean vitrinite reflectance, fuel ratio and H/C ratio. The data suggest that reactivity as determined can be correlated with the mean vitrinite reflectance, fuel ratio and H/C ratio (0.90). The order of reactivity of samples were; Amasra (S1) (R _m= 0.65)>Azdavay (S4) (R _m=0.99)»Armutcuk (S2) (R _m=0.81)»Acenta (S3) (R _m=0.92)>Ac2l2k (S6) (R _m=1.11) Cay (S5) (R _m=1.03)>Sogutozu (S7) (R _m=2.14).     

10MeV 25KW industrial electron LINAC

A 10MeV 25KW plus class electron LINAC was developed for sterilisation of medical devices. The LINAC composed of a standing wave type single cavity prebuncher and a 2m electro-plated travelling wave guide uses a 5MW 2856MHz pulse klystron as an RF source and provides 25KW beam power at the Ti alloy beam window stably after the energy analysing magnet with 10MeV plus-minus 1 MeV energy slit. The practical maximum beam power reached 29 KW and this demonstrated the LINAC as one of the most powerful S-band electron LINACs in the world. The control of the LINAC is fully automated and the “One-Button Operation” is realised, which is valuable for easy operation as a plant system. 2 systems have been delivered and are being operated stably.     

High-performance liquid chromatographic assay of a new non-steroidal anti-inflammatory agent, 2-(10,11-dihydro-10-oxodibenzo[b,f]thiepin-2-yl)propionic acid, in human plasma and urine

A high-performance liquid chromatographic method for the quantitation of a new anti-inflammatory agent, 2-(10,11-dihydro-10-oxodibenzo[b,f]thiepin-2-yl)propionic acid (CN-100; I), has been developed. The assay consists in extracting samples containing I and mefenamic acid, the internal standard, under acidic conditions and analysis by reversed-phase chromatography using ultraviolet detection at 330 nm. Preliminary plasma concentration-time and cumulative urinary excretion profiles from a healthy subject following oral administration of the tablet formulation are presented. This method is simple, sensitive and reproducible and is applicable to studies of the pharmacokinetic behaviour of I in humans.     

Structures of TMC-95A-D: novel proteasome inhibitors from Apiospora montagnei sacc. TC 1093

Four novel proteasome inhibitors, TMC-95A-D (1-4) have been isolated from the fermentation broth of Apiospora montagnei Sacc. TC 1093, isolated from a soil sample. All of the molecular formulas of 1-4 were established as C(33)H(38)N(6)O(10) by high-resolution FAB-MS. Their planar structures were determined on the basis of extensive analyses of 1D and 2D NMR, and degradation studies. Compounds 1-4 have the same planar structures to each other, and are unique highly modified cyclic peptides containing L-tyrosine, L-aspargine, highly oxidized L-tryptophan, (Z)-1-propenylamine, and 3-methyl-2-oxopentanoic acid units. The absolute configuration at C-11 and C-36 of 1-4 was determined based on chiral TLC and HPLC analyses of their chemical degradation products. The ROESY analysis along with (1)H-(1)H coupling constants clarified the absolute stereochemistry at C-6, -7, -8, and -14 of the cyclic moieties. These studies revealed the relationships of 1-4 to be diastereomers at C-7 and C-36.     

Nonlinear stability of circular vortex patches

This paper proves that circular vortex patches in the plane are stable for the nonlinear dynamical system generated by the Euler equations of incompressible fluids. This is achieved by establishing a relative variational principle in terms of either energy or angular momentum. Thus, we exploit and extend Arnold's idea in (1965, 1969) to a nonsmooth setting as well.Research partially supported by DOE contract DE-AT03-82ER12097 to the University of California, Berkeley     

Isolation of new quinidine metabolites and simultaneous determination of quinidine and its metabolites in blood and urine by direct injection HPLC analysis

Summary New quinidine metabolites, including 10,11-dihydrodiol quinidine N-oxide, 10,11-dihydrodiol quinidine and their glucuronides, were found in human urine. A quinidine monitoring HPLC method including these metabolites, is proposed by the direct injection of body fluid samples onto the precolumn for deproteinization followed by reverse phase separation in the analytical column with a column switching technique. The recovery of spiked quinidine and its metabolites in plasma was quantitative (98–102%) with good reproducibility (C.V.: 1.6–4.0%). Several clinical samples such as whole blood and urine were analyzed by the present method.     

Polymer-Supported dicyanoketene acetal as a pi-acid catalyst: monothioacetalization and carbon-carbon bond formation of acetals

Polymeric dicyanoketene acetals (DCKA) were synthesized by copolymerization of styrene and divinylbenzene or ethylene glycol dimethacrylate. These novel polymers could be used successfully as recyclable pi-acid catalysts in monothioacetalization or carbon-carbon bond forming reaction of acetals.