Unless otherwise indicated, all reagents and solvents were purchased from commercial sources and used without further purification. All melting points (°C) were determined on a Tottoli capillary apparatus (Büchi) and are uncorrected; IR spectra were determined in bromoform with a FT/IR 5300 spectrophotometer (Jasco). 1H-NMR and 13C-NMR spectra were respectively recorded, at 200 and 50.3 MHz in CDCl3 or DMSO-d6 solution, using an AC-E series 200 MHz spectrometer (Bruker). Chemical shifts values are given in ppm and referred as the internal standard to tetramethylsilane (TMS). The following abbreviations are used: br s = broad signal, s = singlet, d = doublet, t = triplet, q = quartet, m = multiplet, rt = room temperature. The purity of all compounds screened in biological assays was determined to be >95% by HPLC/MS analysis. Thin layer chromatography was performed on precoated (0.25 mm) silica gel GF254 plates, compounds were detected with 254 nm UV lamp. Column chromatography was performed with silica gel ASTM (230 and 400 mesh, Merck), or with a FLASH40i chromatography module (prepacked cartridge system, Biotage).
Tottoli capillary apparatus
Manufactured by Büchi
The Tottoli capillary apparatus is a laboratory instrument used for the determination of the melting point of solid substances. It allows for the precise and reproducible measurement of the melting point of small samples.
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3 protocols using tottoli capillary apparatus
1
Detailed Spectroscopic Analysis of Organic Compounds
2
Synthesis and Characterization of Organic Compounds
3
Synthesis and Characterization of Organic Compounds
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Reagents, solvents and starting materials were purchased from commercial sources and were used without further purification. Melting points were determined on a Büchi Tottoli capillary apparatus and are uncorrected. The 1 H and 13 C NMR spectra were recorded on a Bruker Avance (500 MHz for 1 H; 125 MHz for 13 C) instrument using deuterated dimethyl sulfoxide (DMSO-d 6 ) as the solvent with tetramethylsilane (TMS) as an internal standard; chemical shifts are reported in δ values (ppm) relative to that of internal TMS. The abbreviations s = singlet, d = doublet, t = triplet, q = quadruplet, p = pentuplet, m = multiplet, qd = quadruplet of doublet, dt = doublet of triplet, dq = doublet of quadruplet, ddt = doublet of doublet of triplet, td = triplet of doublet, and tt = triplet of triplet are used throughout. Elemental analyses (C, H, N, S) were realized on a Thermo Scientific Flash EA 1112 elemental analyzer and were within ±0.4 % of the theoretical values for carbon, hydrogen, and nitrogen. This analytical method certified a purity of ≥95 % for each tested compound. All reactions were routinely checked by TLC on silica gel Merck 60 F254. The synthesis of compounds 14, 17, 19, 20, 21, and 25 was previously described [27] (link).
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