All reactions described were performed under nitrogen atmosphere. Chemicals were at least reagent grade, obtained from Sigma Aldrich (Bornem, Belgium), TCI Europe (Zwijndrecht, Belgium), Activate Scientific (Prien, Germany), Acros (Geel, Belgium) or ChemCollect (Wuppertal, Germany) and used as received. All solvents were obtained from Chemlab (Zedelgem, Belgium) and were at least HPLC-grade. Pre-coated TLC sheets ALUGRAM® Xtra SIL G/UV254 were used to monitor reactions under 254 nm UV-light. Staining of TLC was performed by spraying with either basic aqueous solution of KMnO4 (1.0 g KMnO4, 2.0 g K2CO3, 100 mL H2O) or ninhydrin (1.5g ninhydrin, 3.0 mL acetic acid, 100 mL EtOH) solution and subsequent charring. Purification was performed with silica column chromatography either manually with Machery-Nagel Kieselgel 60 (63–200 μm) or on a Reveleris X2 (Grace) automatic system and accessory pre-packed silica columns. A Waters LCT Premier XE Time of Flight (TOF) mass spectrometer equipped with electrospray ionization (ESI) and a modular Lockspray™ interface was used to obtain high resolution mass spectra. NMR spectra were recorded with a Varian Mercury-300BB (300/75 MHz) spectrometer.
Mercury 300bb 300 75 mhz spectrometer
Manufactured by Agilent Technologies
The Mercury-300BB (300/75 MHz) spectrometer is a compact and versatile nuclear magnetic resonance (NMR) instrument designed for routine analysis. It features a 300 MHz superconducting magnet and a 75 MHz broadband channel, providing high-resolution data acquisition capabilities for a wide range of NMR applications.
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2 protocols using mercury 300bb 300 75 mhz spectrometer
1
Optimized Silica Gel Chromatography Protocol
2
Robust Synthesis of Functionalized Organic Compounds
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All reactions described were performed under an argon atmosphere and at ambient temperature unless stated otherwise. All reagents and solvents were purchased from Sigma-Aldrich (Diegem, Belgium), Acros Organics (Geel Belgium) or TCI Europe (Zwijndrecht, Belgium) and used as received (except THF). THF was dried over sodium/benzophenone. NMR solvents were purchased from Eurisotop (Saint-Aubin, France). Reactions were monitored by TLC analysis using TLC aluminium sheets (Macherey-Nagel, Alugram Sil G/UV 254 ). Detection was by spraying with a solution of (NH 4 ) 6 Mo 7 O 24 •4H 2 O (25 g/L) and (NH 4 ) 4 Ce(SO 4 ) 4 •2H 2 O (10 g/L) in H 2 SO 4 (10 %) followed by charring or immersion in an aqueous solution of KMnO 7 (20 g/L) and K 2 CO 3 (10 g/L) or an ethanolic solution of ninhydrin (2 g/L) and acetic acid (1% v/v) followed by charring. Silica gel column chromatography was performed manually using Grace Davisil 60Å silica gel (40-63 μm) or automated using a Grace Reveleris X2 system and the corresponding flash cartridges. High-resolution spectra were recorded with a Waters LCT Premier XE Mass spectrometer. 1 H-and 13 C-NMR spectra were recorded with a Varian Mercury-300BB (300/75 MHz) spectrometer. Chemical shifts are given in ppm (δ) relative to tetramethylsilane ( 1 H NMR) or the NMR solvent ( 13 C NMR) as an internal standard. In 31
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