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81.
Paolo Davoli 《Tetrahedron》2005,61(18):4427-4436
The enantioselective total synthesis of the actin-targeting metabolite (−)-microcarpalide is described. Key steps include ring-closing metathesis (RCM) for the final construction of the 10-membered lactone framework and stereoselective homologation of boronic esters for the insertion of all stereocentres with the desired absolute configuration. In particular, the acidic fragment was prepared in seven steps from a suitable chiral bromomethane boronate by means of two sequential stereoselective homologations to install the two stereocentres with the correct final R stereochemistry, employing (−)-pinanediol as the chiral director. Subsequent elaboration to the required C7 backbone entailed nucleophilic displacement with a vinyl Grignard reagent, oxidative cleavage of the boronic scaffold and protection-deprotection manipulations. Interestingly, when the tribenzyloxy diene ester resulting from DCC-mediated coupling of the two key synthons was subjected to RCM in the presence of Grubbs' catalyst, the reaction proceeded stereoselectively to yield the desired trans oxecin-2-one, albeit with poor conversion. 相似文献
82.
Vitaliy Petrik 《Tetrahedron letters》2007,48(19):3327-3330
The easy radical trifluoromethylation of a series of 1,3-dicarbonyl compounds with CF3I is described. The reaction occurs in the presence of a nitrogen base and sodium dithionite in CH3CN-H2O solution. Additionally, we report a new access to ammonium triflinates. 相似文献
83.
Summary Clenbuterol has been determined in urine by solidphase extraction on a C18 cartridge, diazotization of the eluate with nitrite, coupling of the diazonium ion with 1-(naphthyl)ethylenediamine, and
separation of the azo dye formed by HPLC with a C18 column and a micellar mobile phase containing 0.1 M sodium dodecyl sulphate, 12%n-butanol and 0.05 M citrate buffer, pH 3. Recoveries higher than 90% were obtained by mixing the samples with a 20% 0.2 M
NaOH before extraction. Limits of detection of 51 and 6.7 ng L−1 were obtained with spectrophotometric and thermal lens spectrometric detection, respectively; respective repeatabilities
were 3.1% (5 μg mL−1) and 5.6% (0.16 μg mL−1). 相似文献
84.
P. Staszczuk J. C. Bazan M. Błachnio D. Sternik N. J. Garcia 《Journal of Thermal Analysis and Calorimetry》2006,86(1):57-68
This paper presents possible applications of thermal analysis, sorptometry
and porosimetry to study physico-chemical properties of Na- and La-montmorillonite
samples, especially for determination of total surface heterogeneity. The
quasi-isothermal thermogravimetric (Q-TG) mass loss and its first derivative
(Q-DTG) curves with respect to temperature and time obtained during programmed
liquid thermodesorption under quasi-isothermal conditions have been used to
study adsorbed layers and heterogeneous properties of the Na- and La-montmorillonites.
Calculations of the desorption energy distribution functions by analytical
procedure using mass loss Q-TG and differential mass loss Q-DTG curves of
thermodesorption under quasi-isothermal conditions of polar and non-polar
liquid vapours preadsorbed on a material surface are presented. Parameters
relating to porosity of samples were determined by sorptometry, mercury porosimetry
and atomic force microscopy (AFM). From nitrogen sorption isotherms from sorptometry
and porosimetry methods, the fractal dimensions of montmorillonites have been
calculated. Moreover, a new approach is proposed to calculate fractal dimensions
of materials obtained from Q-TG curve; this is compared with values obtained
by the above methods. The total heterogeneous properties (energy distribution
function and pore-size distribution functions) of samples studied were estimated.
The radius and pore volume of the tested samples calculated on the basis of
thermogravimetry, sorptometry and porosimetry techniques were compared and
good correlations obtained. 相似文献
85.
Thomas F. Brodasky 《Journal of separation science》1978,1(5):239-244
Two new acyltetramic acids related to streptolydigin have been isolated from fermentations of Streptomyces lydicus. The principal members of this complex were resolved by TLC on silica gel. However, the methods of detection, permanganate spray or bioautography, were not suitable for both crude fermentation broths and purified extracts. Gas chromatography is unsuitable for the detection of either underivatized or silylated streptolydigins. High performance liquid chromatography (HPLC) particularly on triethylaminoethyl cellulose is rapid and sensitive and is the method of choice for the analysis of both crude and purified samples. Using high performance liquid chromatography, two components were detected in the complex, which are not observed using any of the other chromatographic procedures. 相似文献
86.
Methyl methacrylate and butyl methacrylate were polymerized in oil-in-water microemulsions that were stabilized by sodium dodecyl sulphate (SDS). A poly(N-acetylethylenimine) (PNAEI) macromer was also included in the recipe, as a cosurfactant and a comonomer. Polymerizations were initiated by UV-irradiation. The average diameters of latex particles, obtained by STM, were in the range of 17-200 nm. The experimental data evidenced that the particle size was mainly dependent on the SDS/PNAEI ratio. Polymerization yields were around 75-85%. The synthesized copolymers have viscosity average molecular weights in the range of 2.1-2.4×106 and glass transition temperatures of 38.0-43.5°C, lower than those obtained without using PNAEI. The investigation by means of FTIR and 1H-NMR techniques revealed that PNAEI was incorporated into the nanoparticles. 相似文献
87.
Siavosh Mahboobi Andreas Sellmer Thomas Burgemeister Alexei Lyssenko Dieter Schollmeyer 《Monatshefte für Chemie / Chemical Monthly》2004,135(3):333-342
The synthesis of the naturally occurring and biologically active alkaloids 1 and 2, first isolated from the red ascidian Botryllus leachi by Duran et al. [1], is described and the structure proposed for Botryllazine B (1) is confirmed. The analytical data for 2-(p-hydroxybenzoyl)-4-(p-hydroxyphenyl)imidazole (2) are discussed and compared with the literature. With special emphasis of 1H NMR data the tautomerism of aroylimidazolemethanones is described. 相似文献
88.
S. B. Denisova E. G. Galkin V. T. Danilov Yu. I. Murinov 《Chemistry of Natural Compounds》2003,39(3):237-239
Simple sugars were isolated from the ethanol extract of Glycyrrhiza glabra L. root. The component composition of the carbohydrate fraction was established using GC-MS (gas-chromatographic separation and mass-spectrometric analysis). 相似文献
89.
A simple and inexpensive equipment for the optical resolution of enantiomers (and separation of diastereomers) on triacetylcellulose in ethanol at elevated pressure is described. It involves a closed circuit of solvent (pump—column—detector—pump) allowing a continuous chromatography up to 16 cycles without stopping the flow or handling fractions.This useful and versatile method permitting also the determination of enantiomeric purities is illustrated by several examples of centro-, axial- and planarchiral arenes and metallocenes.Herrn Prof. Dr.U. Schmidt, Stuttgart, zum 60. Geburtstag gewidmet. 相似文献
90.
T. A. Vaganova S. Z. Kusov V. I. Rodionov I. K. Shundrina E. V. Malykhin 《Russian Chemical Bulletin》2007,56(11):2239-2246
Amination of pentafluoropyridine, 2,3,5,6-tetrafluoropyridine, 4-chlorotetrafluoropyridine, 3,5-dichlorotrifluoropyridine,
octafluorotoluene, α,α,α,2,3,5,6-heptafluorotoluene, decafluoro-m-xylene, decafluorobiphenyl, hexafluorobenzene, and pentafluorobenzene with liquid ammonia was investigated. Bis-aminodefluorination
temperatures for the majority of substrates were shown to exceed significantly the corresponding temperatures of monoaminodefluorination.
The optimal conditions for selective preparation of mono-and diaminopolyfluoro(het)arenes were elucidated. An efficient method
for isolation of particular polyfluorophenylenediamines from product mixtures formed in nonselective reactions of pentafluorobenzene
and hexafluorobenzene with aqueous ammonia based on complexation with a crown ether is proposed.
Dedicated to the memory of Academician N. N. Vorozhtsov on the occasion of his 100th anniversary.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 11, pp. 2163–2170, November, 2007. 相似文献