All reagents and solvents were of the best grade available supplied by Fluka, Sigma Aldrich, Merck, or Carl Roth and used without further purification. Boc-Lys-OH was obtained from Iris Biotech. Unless otherwise stated, all reactions were performed under argon atmosphere using dry solvents (Sigma Aldrich). Analytical thin-layer chromatography was performed on silica gel 60 plates with fluorescence indicator (254 nm, Merck KGaA). Column chromatography was performed on silica gel 60 (40–63 μm, Macherey-Nagel GmbH & Co. KG) or silica gel C18 end-capped (0.035–0.07 mm, 400–220 mesh, Carl Roth) using solvents of technical grade. Synthesis of PCK (Supplementary Fig. 6 ) was modified according to Gautier and colleagues30 (link). ESI-MS spectra were recorded on VG Fisons with quadrupole analyzer. 1H-NMR spectra were recorded on a BRUKER AV250 or AV400. NMR-Signals were calibrated on solvent signals: 1H-NMR: CDCl3:7.26 ppm; D2O:4.79 ppm. 1H-NMR data are presented as follows: chemical shift in ppm (multiplicity, coupling constant, integration). The following abbreviations are used in reporting NMR-Data: s singlet, d doublet, t triplet, q quartet, dd doublet of doublets, m multiplet.
Av250
Manufactured by Bruker
The AV250 is a compact and versatile nuclear magnetic resonance (NMR) spectrometer designed for routine analysis and research applications. It offers a magnetic field strength of 5.9 Tesla, corresponding to a proton frequency of 250 MHz. The AV250 is equipped with a high-performance superconducting magnet and can be configured with a variety of probe types to accommodate different sample types and experiment requirements.
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Lab products found in correlation
Av 500, by Bruker (2 mentions)
Av 300, by Bruker (2 mentions)
Av 400, by Bruker (1 mentions)
Dry solvents, by Merck Group (1 mentions)
Finnigan mat 95 xp, by Thermo Fisher Scientific (1 mentions)
Emx x band spectrometer, by Bruker (1 mentions)
Avance av400, by Bruker (1 mentions)
Micro cube, by Elementar (1 mentions)
B 545, by Büchi (1 mentions)
Maldi ltq orbitrap mass spectrometer, by Thermo Fisher Scientific (1 mentions)
4 protocols using av250
1
Synthesis of PCK Compound
2
Characterization of Organic Compounds
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The chemicals and solvents used in this study were obtained from
commercial sources. Chemicals were used as such, whereas solvents
were dried or distilled where required. 1H NMR and 13C NMR spectra were obtained by a Bruker spectrometer (AV
250, AV 300, and AV 500) in solvents CDCL3 and DMSO. FTIR spectra
were detected by an ATR apparatus. The high resonance mass spectra
(HRMS) ESI was detected on a device Finnigan MAT 95 XP with an HP-5
capillary column using helium as carrier gas (Thermo Electron Corporation).
The melting point of the compounds was obtained with the use of the
Büchi apparatus. Column chromatography was carried out by using
silica gel 60 A with a mesh size of 60–200. Analytical thin-layer
chromatography was performed on silica gel plates (0.20 mm, 60 A),
and spots were detected through a UV absorbance lamp 254 nm/366 nm.
commercial sources. Chemicals were used as such, whereas solvents
were dried or distilled where required. 1H NMR and 13C NMR spectra were obtained by a Bruker spectrometer (AV
250, AV 300, and AV 500) in solvents CDCL3 and DMSO. FTIR spectra
were detected by an ATR apparatus. The high resonance mass spectra
(HRMS) ESI was detected on a device Finnigan MAT 95 XP with an HP-5
capillary column using helium as carrier gas (Thermo Electron Corporation).
The melting point of the compounds was obtained with the use of the
Büchi apparatus. Column chromatography was carried out by using
silica gel 60 A with a mesh size of 60–200. Analytical thin-layer
chromatography was performed on silica gel plates (0.20 mm, 60 A),
and spots were detected through a UV absorbance lamp 254 nm/366 nm.
3
Synthesis and Characterization of Organophosphorus Compounds
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All manipulations were carried out under dry argon. Solvents were dried by standard procedures. NMR spectra were recorded on Bruker Avance AV 400 or AV 250 instruments ( 1 H: 400.1/ 250.0 MHz, 13 C: 100.5/62.9 MHz, 31 P: 161.9/101.2 MHz); chemical shifts were referenced to ext. TMS ( 1 H, 13 C), 85% H 3 PO 4 (Ξ = 40.480747 MHz, 31 P). Elemental analyses were carried out using an Elementar Micro Cube. Melting Points were determined with a Büchi B-545 melting point apparatus in sealed capillaries. EPR spectra were measured with a Bruker EMX X-band spectrometer. Hyperfine splittings were determined by spectral simulation with the program EasySpin. 12 Quantitative EPR measurements and evaluation of thermochemical data from the spectral data were carried out using the same protocol that had been applied in case of {3c} 2 . A detailed description has been given elsewhere. 4k Chlorophosphane precursors (iPr 2 NPCl 2 , 19 (Me 3 Si) 2 N(iPr 2 N)-PCl, 4a (iPr 2 N) 2 PCl, 20 and (TMP)(iPr 2 N)PCl 21 ) and the diphosphanes {4} 2 , 4j {5} 2 4l and {6} 2 , 10 were prepared as described elsewhere. Diphosphane {7} 2 was prepared by a modification Paper of the reported procdure, 4c using sodium naphthalenide instead of potassium graphite as reducing agent.
4
Analytical Methods for Organic Compounds
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General. Column chromatography: silica gel (60 Å pore size, 0.04-0.063 mm particle size). Proton nuclear magnetic resonance ( 1 H NMR) and carbon nuclear magnetic resonance spectra ( 13 C-NMR) were recorded with Bruker AV 250 ( 1 H: 250 MHz) or Bruker AV 300 ( 1 H: 300 MHz; 13 C: 75.5 MHz) or Bruker AV 500 ( 1 H: 500 MHz; 13 C: 125.8 MHz) NMR spectrometers. Chemical shifts for protons are reported in parts per million (δ scale) and internally referenced to the proton resonances of the solvent (CDCl3: δ 7.26, d6-DMSO: δ 2.50). Chemical shifts for carbon are reported in parts per million (δ scale) and referenced to the carbon resonances of the solvent (CDCl3: δ 77.00, d6-DMSO: δ 39.51). Data are represented as follows: chemical shift, multiplicity (s singlet, bs broad singlet, d doublet, t triplet, q quartet, m multiplet, dd double doublet), coupling constants in Hz, and integration. ESI-MS spectra were obtained on a Fisons VG Plattform II. HRMS spectra were recorded on a MALDI LTQ Orbitrap mass spectrometer from Thermo Scientific.
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