Radial chromatography was performed using a Chromatotron model 7924T (Harrison Research, Palo Alto, CA, USA). Rotors were coated with silicagel 60 PF254 containing gypsum for preparative layer chromatography in 1, 2, or 4 mm thick layers. Silicagel 130–270 Mesh 60 A was used for column chromatography. Melting points were determined in an Optimelt MPA 100 instrument, (Stanford Research Systems, Sunnyvale, CA, USA). NMR spectra of CDCl3 or DMSO-d6 solutions were recorded on Avance DPX 300 MHz (Bruker, Rheinstetten Germany) at 302 K; chemical shifts are reported relative to tetramethylsilane (TMS) or residual solvent peaks. Elemental analyses were performed on a 2400 CHNS/O (Perkin Elmer, Waltham, MA, USA). HRMS spectra were obtained on an 6224 Accurate Mass TOF LC/MS instrument (Agilent, Santa Clara, CA, USA).
Avance dpx 300 mhz
Manufactured by Bruker
Sourced in Germany
The Avance DPX 300 MHz is a nuclear magnetic resonance (NMR) spectrometer. It is designed to perform high-resolution NMR analysis of chemical samples. The core function of the Avance DPX 300 MHz is to generate a strong magnetic field and detect the resonance frequencies of atomic nuclei within the sample, providing detailed information about the chemical structure and composition of the analyzed material.
Automatically generated - may contain errors
Lab products found in correlation
Optimelt mpa 100 instrument, by Stanford Research Systems (1 mentions)
6224 accurate mass tof lc ms instrument, by Agilent Technologies (1 mentions)
Av 400 mhz nmr spectrometer, by Bruker (1 mentions)
Cary winuv software, by Agilent Technologies (1 mentions)
Ltq orbitrap xl, by Thermo Fisher Scientific (1 mentions)
Silica gel 60 f254, by Merck Group (1 mentions)
Silica gel 60, by Merck Group (1 mentions)
Apex 4 instrument, by Bruker (1 mentions)
Dpx 500 mhz, by Bruker (1 mentions)
Dpx 400 mhz, by Bruker (1 mentions)
Silica gel 60 f254 aluminum plates, by Merck Group (1 mentions)
Avance 3 700 mhz, by Bruker (1 mentions)
1100 series lc msd trap system, by Agilent Technologies (1 mentions)
Spectrum one, by PerkinElmer (1 mentions)
5 protocols using avance dpx 300 mhz
1
Radial Chromatography and Spectroscopic Analysis
2
Spectroscopic and Chromatographic Analysis
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TLC analysis was performed using aluminium TLC plates, coated with 0.25 mm silica gel 60 F254 from Merck KGaA. Plates were visualized by UV absorption at 254 nm and/or staining with KMnO4 solution. Flash-column chromatography was performed using silica gel 60 (particle size of 40-63 µm) from Merck KGaA. 1H and 13C NMR spectra were acquired using an Avance DPX-300MHz or AV-400 MHz NMR spectrometer from Bruker at room temperature. Chemical shifts are given in ppm with tetramethylsilane (TMS) or residual solvent (CDCl3: 7.26 ppm for 1H NMR and 77.2 ppm for 13C NMR) as internal standard. Signal multiplicity is described with common abbreviations: singlet (s), broad singlet (sbr), doublet (d), triplet (t), quartet (q), multiplet (m). Coupling constants are given in Hz. See Supplementary Information for detailed chemical synthesis protocols and Supplementary Figs. 12–18 for all 1H NMR spectra. High-resolution mass spectrometry (HRMS) were recorded on a Thermo Scientific LTQ Orbitrap XL. UV absorption spectra were measured using a Cary 3 Bio UV-vis spectrometer (Cary WinUV software, version 3.0, Agilent), scanning from 200 to 550 nm at 1 nm intervals. Scan rate: 120 nm min−1.
3
Comprehensive Analytical Characterization
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All used reagents were purchased from commercial suppliers without further purification. The reactions were carried out in oven-dried or flamed graduated vessels. Solvents were dried and purified by conventional methods before use. All reactions were monitored using Merck aluminum plated pre-coated with silica gel PF254 and detected by visualization of the plate under UV lamp (λ = 254 or 365). Column chromatography was performed using silica gel 60, 0.040–0.063 mm (230–400 mesh). 1H and 13C NMR spectra were recorded on a Bruker Avance DPX-300 MHz and DPX-500 MHz instruments. Splitting patterns are designated as s, singlet; d, doublet; dd, doublet of doublet; t, triplet; q, quartet; m, multiplet; br, broad. Chemical shifts (δ) are given in ppm with reference to TMS as an internal standard. High-resolution mass spectra (HRMS) were measured by Electrospray Ionization (ESI) on a Bruker APEX-IV instrument. The samples were dissolved in acetonitrile and infused using a syringe pump with a flow rate of 120 μL/min. External calibration was conducted using Arginine cluster in a mass range m/z 175–871. For all HRMS data, mass error: 0.00–0.50 mDa.
4
Synthesis of Novel Organic Compounds
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All reagents and solvents were used as purchased without further purification unless stated otherwise. Melting points are uncorrected. Analytical TLC was performed using silica gel 60 F254 aluminum plates (Merck). Flash column chromatography was performed on silica gel 60 (40–63 mm) produced by Merck. NMR spectra were recorded on a Bruker Avance DPX-300 MHz or DPX-400 MHz spectrometer for 1H-NMR, and 75 MHz or 101 MHz for 13C-NMR. Coupling constants (J) are reported in Hertz, and chemical shifts are reported in parts per million relative to CDCl3 (7.26 ppm for 1H and 77.0 ppm for 13C). Mass spectra were recorded at 70 eV with Fison’s VG Pro spectrometer. High-resolution mass spectra were performed with a VG Prospecmass spectrometer and with a Micromass Q-TOF-2™. Protocols for the preparation, physical and spectral data of the intermediates 7 , 8 and 9a–9m are presented in the supplementary materials .
5
Characterization of Platinum Complexes
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Commercial reagent grade chemicals and solvents were used as received without further purification. 1 H-NMR, 195 Pt-NMR and [ 1 H-195 Pt] HSQC spectra were recorded on a Bruker Avance DPX 300 MHz instrument. [ 1 H- 13 C]-HSQC spectra were recorded on a Bruker Avance III 700 MHz instrument. 1 H and 13 C chemical shifts were referenced using the internal residual peak of the solvent (DMSO-d 6 : 2.50 ppm for 1 H and 39.51 ppm for 13 C). 195 Pt NMR spectra were referenced to K 2 PtCl 4 (external standard placed at -1620 ppm with respect to Na 2 [PtCl 6 ]). [17] Electrospray ionisation mass spectrometry (ESI-MS) was performed with an electrospray interface and an ion trap mass spectrometer (1100 Series LC/MSD Trap system Agilent, Palo Alto, CA).
Elemental analyses were carried out with an Eurovector EA 3000 CHN instrument. The Fourier transform infrared spectra were obtained on a Perkin Elmer Spectrum One instrument, using KBr pellets, in the range 4000-200 cm 1 . Intensities of the reported bands are described with s for strong, m for medium and w for weak; broad signals are additionally specified with letter b in front of these abbreviations.
Kiteplatin [18] and cis,trans,cis-[PtCl 2 (OH) 2 (cis-1,4-DACH)] [19] (compound 3) were prepared according to already reported procedures and the given formulation was in good agreement with analytical values (data not shown).
Elemental analyses were carried out with an Eurovector EA 3000 CHN instrument. The Fourier transform infrared spectra were obtained on a Perkin Elmer Spectrum One instrument, using KBr pellets, in the range 4000-200 cm 1 . Intensities of the reported bands are described with s for strong, m for medium and w for weak; broad signals are additionally specified with letter b in front of these abbreviations.
Kiteplatin [18] and cis,trans,cis-[PtCl 2 (OH) 2 (cis-1,4-DACH)] [19] (compound 3) were prepared according to already reported procedures and the given formulation was in good agreement with analytical values (data not shown).
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