Search results for "Trifluoroacetic Acid"
showing 10 items of 34 documents
Star-Shaped Compounds Having 1,3,5-Triazine Cores
2003
The 1,3,5-triazine derivatives 1−4 having styryl or higher oligo(phenylenevinylene) chains in the 2-, 4-, and 6-positions represent star-shaped push-pull compounds. Alkoxy or dimethylamino groups on the peripheral benzene rings, which act as electron donors, and the central 1,3,5-triazine ring, which acts as an electron acceptor, cause intramolecular charge transfer (ICT) to occur in the absorption S0⇄S1. Protonation of the 1,3,5-triazine core enhances the effect, as demonstrated by a bathochromic shift; a secondary protonation on the dimethylamino groups, however, leads to the breakdown of the ICT. Thus, the yellow compound 1d first becomes violet and then colorless upon the addition of tr…
Formation and Reactivity of a Tantalocene Trihydride Containing an Aminoethyl‐Functionalised Ligand
2003
The complex [Cp*{C5H4(CH2CH2NMe2)}TaCl2] (1) was synthesised by reaction of the lithium salt LiC5H4(CH2CH2NMe2) with the tantalum compound [Cp*TaCl3(PMe3)]. Reduction of 1 with NaAl(H)2(OCH2CH2OMe)2 leads to the trihydride derivative [Cp*{C5H4(CH2CH2NMe2)}TaH3] (2). The oxidation of 2 in THF with ferrocenium ion leads to a cationic dihydride intermediate [Cp*{C5H4(CH2CH2NMe2)}TaH2]PF6 (3) with an intramolecular stabilization by the aminoethyl side-chain of the cyclopentadienyl ligand. The hemilabile character of the functionalised cyclopentadienyl ligand was checked by treating 3 with electron-donating ligands (e.g. phosphanes, sulfides, anions); in all cases, no displacement of the amino g…
Elucidation of structure and microheterogeneity of the polypeptide antibiotics paracelsin and trichotoxin A-50 by fast atom bombardment mass spectrom…
1984
Specific and sensitive procedures have been developed which enabled the structure elucidation of the polypeptide antibiotics (peptaibols), paracelsin isolated from Trichoderma reesei, and of trichotoxin A-50 from Trichoderma viride, by fast atom bombardment and field desorption mass spectrometry. Both peptides were found to exhibit a pronounced microheterogeneity by single and multiple exchange of amino acids. Separation by analytical and semipreparative high-performance liquid chromatography (HPLC) on octadecylsilyl-bonded, reversed-phase columns afforded a series of sequence analogues for each polypeptide. Unequivocal molecular weight and sequence identifications were obtained by positive…
Anion-Exchange Properties of Trifluoroacetate and Triflate Salts of N-Alkylammonium Resorcinarenes
2016
The synthesis of N-benzyl- and N-cyclohexylammonium resorcinarene trifluoroacetate (TFA) and triflate (OTf) salt receptors was investigated. Solid-state analysis by single-crystal X-ray diffraction revealed that the N-alkylammonium resorcinarene salts (NARSs) with different upper substituents had different cavity sizes and different affinities for anions. Anion-exchange experiments by mixing equimolar amounts of N-benzylammonium resorcinarene trifluoroacetate and N-cyclohexylammonium resorcinarene triflate, as well as N-benzylammonium resorcinarene triflate and N-cyclohexylammonium resorcinarene trifluoroacetate showed that the NARS with flexible benzyl groups preferred the larger OTf anion…
[(11)C]PR04.MZ, a promising DAT ligand for low concentration imaging: Synthesis, efficient (11)C-O-methylation and initial small animal PET studies.
2009
PR04.MZ was designed as a highly selective dopamine transporter inhibitor, derived from natural cocaine. Its binding profile indicates that [{sup 11}C]PR04.MZ may be suited as a PET radioligand for the non-invasive exploration of striatal and extrastriatal DAT populations. As a key feature, its structural design facilitates both, labelling with fluorine-18 at its terminally fluorinated butynyl moiety and carbon-11 at its methyl ester function. The present report concerns the efficient [{sup 11}C]MeI mediated synthesis of [{sup 11}C]PR04.MZ from an O-desmethyl precursor trifluoroacetic acid salt with Rb{sub 2}CO{sub 3} in DMF in up to 95 {+-} 5% labelling yield. A preliminary {mu}PET-experim…
Experimental and Computational Studies of Hydrogen Bonding and Proton Transfer to [Cp*Fe(dppe)H]
2005
The present contribution reports experimental and computational investigations of the interaction between [Cp*Fe(dppe)H] and different proton donors (HA). The focus is on the structure of the proton transfer intermediates and on the potential energy surface of the proton transfer leading to the dihydrogen complex [Cp*Fe(dppe)(H2)]+. With p-nitrophenol (PNP) a UV/Visible study provides evidence of the formation of the ion-pair stabilized by a hydrogen bond between the nonclassical cation [Cp*Fe(dppe)(H2)]+ and the homoconjugated anion ([AHA]-). With trifluoroacetic acid (TFA), the hydrogen-bonded ion pair containing the simple conjugate base (A-) in equilibrium with the free ions is observed…
Formation and trapping of the thermodynamically unfavoured inverted-hemicucurbit[6]uril
2019
Amplification of a thermodynamically unfavoured macrocyclic product through the directed shift of the equilibrium between dynamic covalent chemistry library members is difficult to achieve. We show for the first time that during condensation of formaldehyde and cis-N,N'-cyclohexa-1,2-diylurea formation of inverted-cis-cyclohexanohemicucurbit[6]uril (i-cis-cycHC[6]) can be induced at the expense of thermodynamically favoured cis-cyclohexanohemicucurbit[6]uril (cis-cycHC[6]). The formation of i-cis-cycHC[6] is enhanced in low concentration of the templating chloride anion and suppressed in excess of this template. We found that reaction selectivity is governed by the solution-based template-a…
Synthesis, Characterization, and Electrochemistry of Open-Chain Pentapyrroles and Sapphyrins with Highly Electron-Withdrawing meso -Tetraaryl Substit…
2017
International audience; A series of open-chain pentapyrroles and sapphyrins with highly electron-withdrawing substituents (i.e., CN, CF3 , or CO2 Me) on the meso-phenyl rings was synthesized and characterized as to the spectral properties, protonation reactions, and electrochemistry in non-aqueous media. The investigated compounds are represented as (Ar)4 PPyH3 and (Ar)4 SapH3 where PPy and Sap correspond to the tri-anion of the open-chain pentapyrrole and sapphyrin, respectively, and Ar=p-CNPh, p-CF3 Ph, or p-CO2 MePh. UV/Vis and 1 H NMR spectroscopy as well as mass spectrometry data are given for the confirmation of the structures for the newly synthesized compounds. An X-ray structure fo…
Determination of biogenic amines in meat by combined ion-exchange capillary gas chromatography
1984
Abstract A procedure is described for the determination of putrescine, cadaverine and histamine in meat. Crude perchloric acid extracts were pre-separated on a weakly acidic cation exchanger and the amines quantified by capillary gas chromatography. The diamines were analysed as trifluoroacetyl derivatives and histamine was converted into N α -trifluoroacetyl-N τ -ethoxycarbonylhistamine. The accuracy of the determination of diamines was examined by a precipitation pre-separation method and by mass fragmentometric quantification. The proposed procedure allows the sensitive, sufficiently precise and highly specific determination of putrescine and cadaverine in meat.
Analysis of neuropeptide Y and its metabolites by high-performance liquid chromatography-electrospray ionization mass spectrometry and integrated sam…
2000
A novel restricted access cation exchanger with sulphonic acid groups at the internal surface was proven to be highly suitable in the sample clean up of peptides on-line coupled to HPLC-electrospray ionization (ESI)-MS. Neuropeptide Y (NPY) and several of its fragments in plasma were subjected to the sample clean-up procedure. The peptides were eluted by a step gradient from the restricted access column, applying 10 mM phosphate buffer pH 3.5 from 5 to 20% (v/v) of acetonitrile with 1 M NaCl and transferred to a Micra ODS II column (33x4.6 mm). The separation of the peptides and their fragments was performed by a linear gradient from 20 to 60% (v/v) acetonitrile in water with 0.1% formic ac…