Silica gel 60f254 sheets

Reagents and solvents used in this study were of analytical grade purity and purchased from Sigma-Aldrich Chemicals (Buchs, Switzerland) and Alfa Aesar (Karlsruhe, Germany). The progress of all reactions was checked by thin layer chromatography (TLC) using precoated Silica Gel 60F₂₅₄ sheets (Merck, Darmstadt, Germany). The spots on plates were visualized under UV light (254 nm). Melting points (m.p.) were determined using an MPM-H1 melting point apparatus (Schorpp Gerätetechnik, Überlingen, Germany) and are uncorrected. Elemental analyses for C, H, N and S were carried out on a Vario El CHNS instrument (Hanau, Germany). FT-IR spectra were recorded on a JASCO FT-IR-6100 spectrophotometer (Cremella, Italy). ¹H-NMR and ¹³C-NMR analyses were performed on an Avance NMR spectrometer (Bruker, Karlsruhe, Germany), operating at 500 MHz and 125 MHz respectively, in DMSO-d₆, using tetramethylsilane (TMS) as internal standard. Chemical shifts (δ values) are expressed in parts per million (ppm). M + 1 peaks were determined on an Agilent 1100 series and an Agilent Ion Trap SL mass spectrometer (Santa Clara, CA, USA), operating at 70 eV.

Analytical thin-layer chromatography (TLC) was carried out on Merck Silica Gel 60F254 sheets (Darmstadt, Germany). It was employed for monitoring the purification process and the reaction progress of new compounds. The elution was using a mixture of n-hexane: EtOAc = 4:1 and UV light (254 nm) together with molybdophosphoric acid and heating for visualization. Preparative chromatography was performed using Merck silica gel 60 and Sephadex LH-20 (25–100 μm; Aldrich, Santiago, Chile). Solvents and fractions were concentrated in a Büchi R100 rotavap. Solvents used in this study were distilled before use and dried over appropriate drying agents.

Analytical thin-layer chromatography (TLC) was carried out on Merck Silica Gel 60F254 sheets (Darmstadt, Germany). It was employed for monitoring the purification process and the reaction progress of new compounds, using a mixture of n-hexane: EtOAc = 1:1 and molybdophosphoric acid for visualization. Preparative chromatography was performed using Merck silica gel 60 (CC) and Sephadex LH-20 (25−100 μm; Aldrich, Santiago, Chile). Solvents and fractions were concentrated in vacuo using a Büchi R100 rotavap. Solvents used in this study were distilled before use and dried over appropriate drying agents.