For reaction progress and purity control TLC was performed on TLC silica gel 60 F254 aluminium sheets 20 × 20 cm from Merck. Visualisation was performed with a 254 nm UV lamp (low pressure Hg-Lamp from DESAGA) or by using an aqueous solution of KMnO4 (1.0 g KMnO4, 6.6 g K2CO3, 0.2 g NaOH in 100 ml water). The purification of the products was carried out by column chromatography with Geduran® Si 60 Silicagel (40–63 μm) from Merck.
Geduran si 60 silicagel
Manufactured by Merck Group
Sourced in Germany
Geduran® Si 60 Silicagel is a high-purity silica gel product designed for use in various laboratory applications. It is a granular, porous material with a high surface area, making it suitable for applications such as chromatography, desiccation, and adsorption processes.
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Lab products found in correlation
Tlc silica gel 60 f254 aluminium sheets, by Merck Group (1 mentions)
Tlc si60 f254, by Merck Group (1 mentions)
Merck silica gel 60 f254, by Merck Group (1 mentions)
Agotf, by Merck Group (1 mentions)
Spectrum one spectrophotometer, by PerkinElmer (1 mentions)
Ph3p aucl, by Merck Group (1 mentions)
Agbf4, by Merck Group (1 mentions)
Avance 300, by Bruker (1 mentions)
3 protocols using geduran si 60 silicagel
1
TLC Visualization and Column Chromatography
2
General Organic Synthesis Techniques
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Reactions and characterisations were performed by default with non-degassed solvents, reagents and building blocks, that were purchased from standard commercial sources. Anhydrous solvents obtained in septum-capped bottles and analytical grade or higher quality solvents were used without purification. Industrial grade solvents were distilled prior to use. Unless otherwise stated, reactions were performed at room temperature without precautions regarding air or moisture and were stirred using magnetic Teflon®-coated stir bars. Air or moisture sensitive reactions were conducted in dry Schlenk glassware. Flash column chromatography was performed on Geduran® Si 60 silica gel from Merck GmbH, Darmstadt (Germany) or using a Biotage® Select automated column chromatography system with manufacturer’s cartridges from Biotage GmbH, Uppsala (Sweden). Thin layer chromatography to monitor reactions and determine Rf-values was performed on silica coated aluminium sheets with fluorescent indicator (TLC Si 60 F254 from Merck GmbH, Darmstadt, Germany) with visualisation by UV irradiation (254 nm/360 nm) or staining with KMnO4 solution (3.0 g KMnO4, 20 g K2CO3, 0.30 g KOH, 0.30 L H2O).
3
Gold(I) Catalyzed Organic Synthesis
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All reactions were carried out under argon atmosphere in dried glassware. Toluene and benzene were dried and freshly distilled from sodium. Acetonitrile was dried and freshly distilled from CaH2. (Ph3P)AuCl, AgOTf, AgBF4 and CuI were purchased from Sigma-Aldrich ® , in ≥99.9%, ≥99.95% and 98% purity respectively. (Ph3P)2PdCl2 was prepared from PdCl2 and PPh3.
Reactions were monitored by TLC with Merck ® Silica gel 60 F254. Purifications by flash chromatography were carried out using Merck ® Geduran ® Si 60 silica gel (40-63 µm). 1 H NMR spectra were recorded on a Bruker ® Avance 300 (300 MHz) NMR spectrometer, using CDCl3 as solvent. Data, reported using Me4Si (δH = 0.00 ppm) as internal reference, were as follows (in order): chemical shift (δ in ppm relative to Me4Si), multiplicity (s, d, t, q, m, br for singlet, doublet, triplet, quartet, multiplet, broad) and coupling constants (J in Hz). 13 C NMR was recorded at 75 MHz on the same instrument, using the CDCl3 solvent peak at (δC = 77.16 ppm) as reference. 19 F NMR was recorded at 282 MHz on the same instrument, using the CClF3 peak at (δF = 0.0 ppm) as internal reference. Mass spectra were obtained on a Hewlett Packard (engine 5988A) by direct inlet at 70eV. IR spectra were recorded on a Perkin-Elmer Spectrum One spectrophotometer. Melting points were uncorrected.
Reactions were monitored by TLC with Merck ® Silica gel 60 F254. Purifications by flash chromatography were carried out using Merck ® Geduran ® Si 60 silica gel (40-63 µm). 1 H NMR spectra were recorded on a Bruker ® Avance 300 (300 MHz) NMR spectrometer, using CDCl3 as solvent. Data, reported using Me4Si (δH = 0.00 ppm) as internal reference, were as follows (in order): chemical shift (δ in ppm relative to Me4Si), multiplicity (s, d, t, q, m, br for singlet, doublet, triplet, quartet, multiplet, broad) and coupling constants (J in Hz). 13 C NMR was recorded at 75 MHz on the same instrument, using the CDCl3 solvent peak at (δC = 77.16 ppm) as reference. 19 F NMR was recorded at 282 MHz on the same instrument, using the CClF3 peak at (δF = 0.0 ppm) as internal reference. Mass spectra were obtained on a Hewlett Packard (engine 5988A) by direct inlet at 70eV. IR spectra were recorded on a Perkin-Elmer Spectrum One spectrophotometer. Melting points were uncorrected.
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