Search results for "Reagent"

Alkylation of acidic organic compounds for gas chromatographic analysis

1973

A new alkylation method is proposed. Organic solutions of fatty acids, phenols or barbituric acids are refluxed with an alkylating reagent and solid K2CO3. The reaction mixture is injected directly into the gas chromatograph. The scope of this convenient method for quantitative and qualitative analyses is considerable as different classes of alkylating agents can be used.

Combretastatin Analogs via Hydration of Stilbene Derivatives

1993

Hydration of the double bond of some stilbene congeners of Picea abies bark by TiCl4·NaBH4 reagent is described. Five racemic 1,2-diphenylethanol derivatives (9–13), structurally related to (R)-(·)-combretastatin [(R)-1], have been obtained and characterized mainly by 13C- and 1H-NMR as well as mass spectrometry. The antileukemic activity of each compound has preliminarily been tested by the mouse leukemia L1210 system. Compound 10 has been synthesized by Friedel-Crafts acylation.

Enhanced spectrophotometric determination of nicotinic acid in a sodium dodecyl sulphate micellar medium.

1994

The spectrophotometric determination of pyridine and pyridine derivatives by means of the König reaction was studied in micellar media of sodium dodecyl sulphate (SDS), N-cetylpyridinium chloride and Triton X-100. The sensitivity was largely increased in SDS micellar medium. The attack of the pyridine ring with cyanogen bromide to produce a glutaconic aldehyde was not affected by the presence of SDS, but the yield of the coupling reaction with an arylamine to produce a polymethine dye was largely increased. In the SDS micellar medium, aniline was superior to other coupling reagents. The limits of detection (LODs) were 6 x 10(-7), 1 x 10(-6) and 5 x 10(-7)M for pyridine, pyrrol-ylmethylpyrid…

Characterization of proteinaceous glues in old paintings by separation of the o-phtalaldehyde derivatives of their amino acids by liquid chromatograp…

2005

A HPLC-fluorescence method for characterization of proteinaceous glues from binding media used in pictorial works of art prior to conservation or restoration treatment is proposed. Fluorescence derivatization of amino acids released by acid hydrolysis of standard proteins is studied. The derivatization reagent was o-phtalaldehyde with 2-mercaptoethanol as catalyst. Mobile phase was a programmed gradient among two eluents (water buffered at pH 5.8 wit 5% THF, and methanol) and is able to satisfactorily resolve the amino acid derivatives in 45min. Peak area ratios among amino acid derivatives and the leucine derivative are useful to characterize the proteins. The method shows good sensitivity…

Modular Hemisyntheses of Boronato- and Trifluoroborato-SubstitutedL-NHBoc Amino Acid and Peptide Derivatives

2013

Modular hemisyntheses of boronato- and trifluoroborato-substituted amino acid and peptide derivatives by using Wittig and C–H iridium-catalyzed borylation as key reactions, are described. Amino ester precursors bearing an aromatic moiety on a lateral chain were prepared by reaction of a new L-NHBoc-amino acid Wittig reagent with the corresponding aromatic aldehydes. After esterification and hydrogenation, the borylation of amino esters was achieved with yields up to 82 % by using the catalysed reaction of bis(pinacolato) diborane reagent (B2Pin2) in the presence of an iridium complex. Interestingly, this iridium-catalyzed borylation was also performed with a dipeptide in 78 % yield. Finally…

Conjugate Alkynylation of Electrophilic Double Bonds. From Regioselectivity to Enantioselectivity

2018

This review surveys the historical efforts addressed toward the development of the conjugate alkynylation reaction. The regio- and enantioselective conjugate alkynylation of electron-deficient double bonds, most commonly unsaturated carbonyl compounds, has been an elusive reaction for a long time. Intensive research during the last decades has resulted in the identification of a number of effective reagents and catalysts to perform this reaction. Non-stereoselective conjugate alkynylation of unsaturated carbonyl compounds was first achieved by using preformed alkynyl organometallics and later with terminal alkynes under catalytic conditions. These methods paved the way for the development o…

Cu(ii)-alginate-based superporous hydrogel catalyst for click chemistry azide-alkyne cycloaddition type reactions in water.

2020

A novel sustainable hydrogel catalyst based on the reaction of sodium alginate naturally extracted from brown algae Laminaria digitata residue with copper(II) was prepared as spherical beads, namely Cu(II)-alginate hydrogel (Cu(II)-AHG). The morphology and structural characteristics of these beads were elucidated by different techniques such as SEM, EDX, BET, FTIR and TGA analysis. Cu(II)-AHG and its dried form, namely Cu(II)-alginate (Cu(II)-AD), are relatively uniform with an average pore ranging from 200 nm to more than 20 μm. These superporous structure beads were employed for the copper catalyzed [3 + 2] cycloaddition reaction of aryl azides and terminal aryl alkynes (CuAAC) via click …

Iron-Catalyzed C(sp2)-C(sp3) Cross-Coupling of Alkyl Grignard Reagents with Polyaromatic Tosylates

2017

Cover Feature: Metal‐ and Reagent‐Free Electrochemical Synthesis of Alkyl Arylsulfonates in a Multi‐Component Reaction (Chem. Eur. J. 38/2020)

2020

Impact of O → S Exchange in Ferrocenyl Amides on the Structure and Redox Chemistry

2014

The conformations and redox chemistry of ferrocenyl amides have been investigated in considerable depth in the last few years, while ferrocenyl thioamides have attracted less interest so far, although distinctly different conformations and reactivity patterns are expected. Monoferrocenyl amides Fc-NHC(O)CH3 (1) and 1,1′-CH3O(O)C-Fn-NHC(O)CH3 (2) and diferrocenyl amides Fc-NHC(O)-Fc (5) and Fc-NHC(O)-Fn-NHC(O)CH3 (6) are easily transformed into the corresponding thioamides (3, 4, 7, 8) by treatment with Lawesson’s reagent (2,4-bis(p-methoxyphenyl)-1,3-dithiaphosphetane-2,4-disulfide) (Fc = Fe(C5H4)(C5H5), Fn = Fe(C5H4)2). The thioamide conformations (cis/trans) in 3, 4, 7, and 8 and the hydr…