Triterpenoid saponins from the roots of Acanthophyllum gypsophiloides Regel

• Elena A. Khatuntseva,
• Vladimir M. Men’shov,
• Alexander S. Shashkov,
• Yury E. Tsvetkov,
• Rodion N. Stepanenko,
• Raymonda Ya. Vlasenko,
• Elvira E. Shults,
• Genrikh A. Tolstikov,
• Tatjana G. Tolstikova,
• Dimitri S. Baev,
• Vasiliy A. Kaledin,
• Nelli A. Popova,
• Valeriy P. Nikolin,
• Pavel P. Laktionov,
• Anna V. Cherepanova,
• Tatiana V. Kulakovskaya,
• Ekaterina V. Kulakovskaya and
• Nikolay E. Nifantiev

Beilstein J. Org. Chem. 2012, 8, 763–775, doi:10.3762/bjoc.8.87

• Bruker micrоTOF II instrument by using electrospray ionization (ESI) [28]. The measurements were done in a positive-ion mode (interface capillary voltage: 4500 V) or in a negative-ion mode (3200 V); mass range from m/z 50–3000 Da; external or internal calibration was achieved with electrospray calibrant

Enantioselective supramolecular devices in the gas phase. Resorcin[4]arene as a model system

• Caterina Fraschetti,
• Matthias C. Letzel,
• Antonello Filippi,
• Maurizio Speranza and
• Jochen Mattay

Beilstein J. Org. Chem. 2012, 8, 539–550, doi:10.3762/bjoc.8.62

• , even in the gas phase. The most recent advances in this field include several gas-phase investigations: (i) The size and structure selectivity of tetraethyl and tetraphenyl resorcin[4]arenes in the recognition of mono, di-, and oligosaccharides by electrospray coupled with Fourier transform ion

• the attention will be focussed on the most recent results obtained by our group with this particular kinetic method. Methodology The proton-bound [M∙H∙G]+ aggregates (M: chiral hosting resorcin[4]arene; G: guest biomolecule) were generated by electrospray ionization (ESI) of M/G methanolic mixtures

Branching out at C-2 of septanosides. Synthesis of 2-deoxy-2-C-alkyl/aryl septanosides from a bromo-oxepine

• Supriya Dey and
• Narayanaswamy Jayaraman

Beilstein J. Org. Chem. 2012, 8, 522–527, doi:10.3762/bjoc.8.59

• Merck plates coated with silica gel GF254 (0.25 mm). Silica gel (230–400 mesh) was used for column chromatography. Optical rotations were recorded on a JASCO Model P-1020 polarimeter at the sodium D line at 24 °C. High-resolution mass spectra were obtained from a Q-TOF instrument by the electrospray

Mutational analysis of a phenazine biosynthetic gene cluster in Streptomyces anulatus 9663

• Orwah Saleh,
• Katrin Flinspach,
• Lucia Westrich,
• Andreas Kulik,
• Bertolt Gust,
• Hans-Peter Fiedler and
• Lutz Heide

Beilstein J. Org. Chem. 2012, 8, 501–513, doi:10.3762/bjoc.8.57

• B in 15 min (solvent A: water/formic acid (999:1); solvent B: acetonitrile/formic acid (999.4:0.6)). Detection was carried out at 230, 260, 280, 360, and 435 nm. Electrospray ionization (positive and negative ionization) in Ultra Scan mode with capillary voltage of 3.5 kV and drying gas temperature

Self-assembly of Ru₄ and Ru₈ assemblies by coordination using organometallic Ru(II)₂ precursors: Synthesis, characterization and properties

• Sankarasekaran Shanmugaraju,
• Dipak Samanta and
• Partha Sarathi Mukherjee

Beilstein J. Org. Chem. 2012, 8, 313–322, doi:10.3762/bjoc.8.34

• salts in high yields and were characterized fully by multinuclear (1H, 13C and 19F) NMR, infrared (IR) and electrospray ionization mass spectrometry (ESIMS). In addition, the molecular structure of macrocycle 2a was established unequivocally by single-crystal X-ray diffraction analysis and adopts a

• information about the exact composition and nuclearity of the final products. Electrospray ionization mass spectrometry (ESIMS) can be used as a soft-ionization method to elucidate the exact composition of the product [12]. The ESIMS analysis confirmed the formation of the rather unexpected [2 + 1] self

Fluorescent hexaaryl- and hexa-heteroaryl[3]radialenes: Synthesis, structures, and properties

• Antonio Avellaneda,
• Courtney A. Hollis,
• Xin He and
• Christopher J. Sumby

Beilstein J. Org. Chem. 2012, 8, 71–80, doi:10.3762/bjoc.8.7

• elemental analyses. Low resolution electrospray ionisation mass spectra (ESIMS) were recorded on a Finnigan LCQ mass spectrometer. Samples were dissolved in HPLC grade methanol or acetonitrile with a concentration of 0.01 mg/cm3. High resolution electrospray ionisation mass spectroscopy (ESI-HRMS) was

Valence isomerization of cyclohepta-1,3,5-triene and its heteroelement analogues

• Helen Jansen,
• J. Chris Slootweg and
• Koop Lammertsma

Beilstein J. Org. Chem. 2011, 7, 1713–1721, doi:10.3762/bjoc.7.201

• + 2] cycloadditions of the in situ generated singlet phosphinidene 35 with olefins or acetylenes (Scheme 7) [5][6][7][8][9]. This approach has even lead to the detection of the transient phosphinidene species by employing electrospray ionization tandem mass spectrometry (ESIMS/MS); its gas-phase

Impact of the level of complexity in self-sorting: Fabrication of a supramolecular scalene triangle

• Kingsuk Mahata and
• Michael Schmittel

Beilstein J. Org. Chem. 2011, 7, 1555–1561, doi:10.3762/bjoc.7.183

• characterised as received, by means of mass spectrometry, 1H NMR, diffusion-ordered spectroscopy (DOSY), differential pulse voltammetry (DPV) and elemental analysis. The electrospray ionisation mass spectrum (ESI-MS) of the reaction mixture suggests clean formation of the triangular species T = [Cu2Zn(5)(6)(7

• and distilled prior to use. NMR measurements were carried out on a Bruker Avance 400 MHz spectrometer with the deuterated solvent as the lock and residual solvent as the internal reference. Electrospray ionisation mass spectra (ESI-MS) were recorded on a Thermo-Quest LCQ Deca. Differential pulse

A new phenylethyl alkyl amide from the Ambrostoma quadriimpressum Motschulsky

• Guolei Zhao,
• Chao Yang,
• Bing Li and
• Wujiong Xia

Beilstein J. Org. Chem. 2011, 7, 1342–1346, doi:10.3762/bjoc.7.158

• ) ionization at 70 eV. 1H NMR spectra were obtained at 400 MHz on a Bruker AV-400 instrument. 13C NMR spectra were recorded at 100 MHz. High-resolution mass spectra were recorded on an Agilent 1200-6520 Q-TOF electrospray mass spectrometer. Isolation of (10R)-10-hydroxy-N-phenethyloctadecanamide (1

A simple and convenient one-pot synthesis of substituted isoindolin-1-ones via lithiation, substitution and cyclization of N'-benzyl-N,N-dimethylureas

• Keith Smith,
• Gamal A. El-Hiti,
• Amany S. Hegazy and
• Benson Kariuki

Beilstein J. Org. Chem. 2011, 7, 1219–1227, doi:10.3762/bjoc.7.142

• impact (EI) at 70 eV and chemical ionization (CI) at 50 eV by the use of NH3 as ionization gas. Atmospheric pressure chemical ionization (APCI) mass spectra were measured on a Waters LCT Premier XE instrument. Electrospray (ES) analyses were performed on a ZQ4000 spectrometer in positive and negative

Single enantiomer synthesis of α-(trifluoromethyl)-β-lactam

• Václav Jurčík,
• Alexandra M. Z. Slawin and
• David O'Hagan

Beilstein J. Org. Chem. 2011, 7, 759–766, doi:10.3762/bjoc.7.86

• measured using a Perkin Elmer Model 341 polarimeter. Mass spectrometric (m/z) data was acquired by electrospray ionisation (ESI). High resolution mass analyses were recorded on a Micromass LCT TOF mass spectrometer using ES ionisation in positive ion mode. General aza-Michael procedure NaHCO3 (840 mg, 10.0

Synthesis and self-assembly of 1-deoxyglucose derivatives as low molecular weight organogelators

• Guijun Wang,
• Hao Yang,
• Sherwin Cheuk and
• Sherman Coleman

Beilstein J. Org. Chem. 2011, 7, 234–242, doi:10.3762/bjoc.7.31

• using a 400 MHz Varian NMR spectrometer. High resolution mass spectrometry data were measured on the Q-Tof of the Mass Spectrometry lab at the University of Illinois after the low resolution masses were confirmed. The ionization technique used was ESI (electrospray ionization). Melting points were

Surfactant catalyzed convenient and greener synthesis of tetrahydrobenzo[a]xanthene-11-ones at ambient temperature

• Pravin V. Shinde,
• Amol H. Kategaonkar,
• Bapurao B. Shingate and
• Murlidhar S. Shingare

Beilstein J. Org. Chem. 2011, 7, 53–58, doi:10.3762/bjoc.7.9

• cm−1. 1H NMR and 13C NMR spectra were recorded on an NMR spectrometer AC200 in CDCl3, chemical shifts (δ) are given in ppm relative to TMS. Mass spectra were taken on a Macro mass spectrometer (Waters) by the electrospray method (ES). Optical microscopy measurements: A drop of the turbid reaction

Design and synthesis of a cyclitol-derived scaffold with axial pyridyl appendages and its encapsulation of the silver(I) cation

• Pierre-Marc Léo,
• Christophe Morin and
• Christian Philouze

Beilstein J. Org. Chem. 2010, 6, 1022–1024, doi:10.3762/bjoc.6.115

• Information File 1). However, in the absence of characteristic signals for Ag(I)-complex (even at low temperature: −50 °C) NMR methods cannot be used for the determination of the complex stability constant. The electrospray mass spectrum (from the very solution contained in the NMR tube) revealed a 1:1

• (ellipsoids are drawn at the 50% probability level and H atoms are omitted for clarity). Supporting Information Supporting Information features experimental procedures, 1H NMR and 13C NMR spectra; electrospray mass spectrum and the crystal structure of the Ag complex. Supporting Information File 158

Molecular recognition of organic ammonium ions in solution using synthetic receptors

• Andreas Späth and
• Burkhard König

Beilstein J. Org. Chem. 2010, 6, No. 32, doi:10.3762/bjoc.6.32

Templated versus non-templated synthesis of benzo-21-crown-7 and the influence of substituents on its complexing properties

• Wei Jiang and
• Christoph A. Schalley

Beilstein J. Org. Chem. 2010, 6, No. 14, doi:10.3762/bjoc.6.14

• coupling constants (J) are in Hertz. The following abbreviations were used for signal multiplicities: s, singlet; d, doublet; t triplet; m, multiplet. Electrospray-ionization time-of-flight high-resolution mass spectrometry (ESI-TOF-HRMS) experiments were conducted on an Agilent 6210 ESI-TOF, Agilent

• Technologies and a Varian/IonSpec QFT-7 FTICR (Fourier-transform ion-cyclotron-resonance) mass spectrometer equipped with a superconducting 7 Tesla magnet and a micromass Z-spray Electrospray-ionization (ESI) ion source utilizing a stainless steel capillary with a 0.75 mm inner diameter. 2-{2-[2-(2-{2-[2-(2

Synthesis of phosphonate and phostone analogues of ribose-1-phosphates

• Pitak Nasomjai,
• David O'Hagan and
• Alexandra M. Z. Slawin

Beilstein J. Org. Chem. 2009, 5, No. 37, doi:10.3762/bjoc.5.37

• . Infra red (IR) spectra were recorded on Nicolet Avatar 360 FT-IR. High resolution mass spectrometry (HRMS) was carried out using a Micromass LCT (Manchester, UK) mass spectrometer with electrospray ionization (ESI) operating in positive and negative modes. Optical rotations were measured on Perkin-Elmer

Synthesis of rigidified flavin–guanidinium ion conjugates and investigation of their photocatalytic properties

• Harald Schmaderer,
• Mouchumi Bhuyan and
• Burkhard König

Beilstein J. Org. Chem. 2009, 5, No. 26, doi:10.3762/bjoc.5.26

• 35–70 μm, 60 Å from Acros. NMR spectra were recorded at a Bruker Avance 300 spectrometer (300 MHz) or at a Bruker Avance 600 spectrometer (600 MHz). Electrospray ionisation (ES-MS) mass spectra were measured on ThermoQuest Finnigan TSQ 7000 spectrometer. High resolution mass spectrometry (HRMS) was

Synthesis of methylenebisamides using CC- or DCMT- activated DMSO

• Qiang Wang,
• Lili Sun,
• Yu Jiang and
• Chunbao Li

Beilstein J. Org. Chem. 2008, 4, No. 51, doi:10.3762/bjoc.4.51

• DMSO-d6 or CDCl3 (13C). Mass spectra were obtained using an LCQ Advantage MAX ion trap mass spectrometer equipped with electrospray ionization (ESI) ion source or a Thermo Finnigan TRACE-DSQ spectrometer. Elemental analyses for C, H and N were performed on a Yanaco CHNCORNER MF-3 elemental analyzer

Synthesis of imidazol- 1-yl-acetic acid hydrochloride: A key intermediate for zoledronic acid

• Santosh Kumar Singh,
• Narendra Manne,
• Purna Chandra Ray and
• Manojit Pal

Beilstein J. Org. Chem. 2008, 4, No. 42, doi:10.3762/bjoc.4.42

• Avance 300 spectrometer (300 MHz). Electrospray (ES+) mass spectra were acquired on an ion trap mass spectrometer. Preparation of imidazol-1-yl-acetic acid tert-butyl ester (2) To a solution of imidazole (10.0 g, 0.15 mol) in ethyl acetate (160 mL) was added powdered K2CO3 (29.0 g, 0.21 mol) followed by

The first preparative solution phase synthesis of melanotan II

• Vladimir V. Ryakhovsky,
• Georgy A. Khachiyan,
• Nina F. Kosovova,
• Elena F. Isamiddinova and
• Andrey S. Ivanov

Beilstein J. Org. Chem. 2008, 4, No. 39, doi:10.3762/bjoc.4.39

• synthesized product and melanotan II purchased from a commercial source. Electrospray injection mass spectrometry of both samples demonstrated two characteristic peaks with m/z 512 and 1024, corresponding to [M+2H]2+ and [M+H]+ respectively. Conclusion In conclusion, we have developed the first solution phase

Synthesis of (S)-1-(2-chloroacetyl)pyrrolidine- 2-carbonitrile: A key intermediate for dipeptidyl peptidase IV inhibitors

• Santosh K. Singh,
• Narendra Manne and
• Manojit Pal

Beilstein J. Org. Chem. 2008, 4, No. 20, doi:10.3762/bjoc.4.20

• applications in the design and synthesis of novel DPP-IV inhibitors for the potential treatment of type-II diabetes. Experimental General methods All the compounds synthesized were characterized by NMR, IR and MS spectra. 1H NMR spectra were recorded on a Bruker Avance 300 spectrometer (300 MHz). Electrospray