Sepacor chromatography module

All melting points were taken on a Büchi-Tottoly capillary apparatus and are uncorrected. IR spectra were determined in bromoform with a Shimadzu FT/IR 8400S spectrophotometer. ¹H and ¹³C NMR spectra were measured at 200 and 50.0 MHz, respectively, in DMSO-d₆ solution, using a Bruker Avance II series 200 MHz spectrometer. Column chromatography was performed with Merck silica gel 230–400 mesh ASTM or with Büchi Sepacor chromatography module (prepacked cartridge system). Elemental analyses (C, H, N) were within ±0.4% of theoretical values and were performed with a VARIO EL III elemental analyser. Purity of all the tested compounds was greater than 95%, determined by HPLC (Agilent 1100 Series).

All melting points were taken on a Büchi melting point M-560 apparatus. IR spectra were determined in bromoform with a Shimadzu FT/IR 8400S spectrophotometer. ¹H and ¹³C NMR spectra were measured at 200 and 50.0 MHz, respectively, in DMSO-d₆ or CDCl₃ solution using a Bruker Avance II series 200 MHz spectrometer. Column chromatography was performed with Merck silica gel (230 − 400 mesh ASTM) or a Büchi Sepacor chromatography module (prepacked cartridge system). Elemental analyses (C, H, N) were within ± 0.4% of theoretical values and were performed with a VARIO EL III elemental analyzer. The purity of all the tested compounds was > 95%, determined by HPLC (Agilent 1100 series).
Compounds 9a–e were prepared according to published procedure (Barreca et al. 2022a (link)).

All melting points were taken on a Büchi-Tottoly capillary apparatus (Büchi, Cornaredo, Italy) and are uncorrected. IR spectra were determined in bromoform with a Shimadzu FT/IR 8400S spectrophotometer (Shimadzu Corporation, Milan, Italy). ¹H and ¹³C NMR spectra were measured at 200 and 50.0 MHz, respectively, in DMSO-d₆ solution, using a Bruker Avance II series 200 MHz spectrometer (Bruker, Milan, Italy). Column chromatography was performed with Merck silica gel 230–400 mesh ASTM or with a Büchi Sepacor chromatography module (prepacked cartridge system). Elemental analyses (C, H, N) were within ± 0.4% of theoretical values and were performed with a VARIO EL III elemental analyzer (Elementar, Langenselbold, Germany). Purity of all the tested compounds was greater than 95%, determined by HPLC (Agilent 1100 Series). Mass spectra of final compounds were performed using a Mariner™ mass spectrometer, Applied Biosystems (Foster City, CA, USA). A Harvard model 11 syringe pump (Holliston, MA, USA) was used to infuse the sample solutions. The ESI source was operated in positive ion mode with an electrospray voltage of 4.5 kV. Compounds 1a–o were characterized only by ¹H NMR spectra due to their poor solubility.

All melting points were taken on a Büchi-Tottoly capillary apparatus (Büchi, Cornaredo, Italy) and are uncorrected. IR spectra were determined in bromoform with a Shimadzu FT/IR 8400S spectrophotometer (Shimadzu Corporation, Milan, Italy). ¹H and ¹³C NMR spectra were measured at 200 and 50.0 MHz, respectively, in DMSO-d₆ solution, using a Bruker Avance II series 200 MHz spectrometer (Bruker, Milan, Italy). Column chromatography was performed with Merk silica gel 230–400 mesh ASTM or with Büchi Sepacor chromatography module (prepacked cartridge system). Elemental analyses (C, H, and N) were within ± 0.4% of theoretical values. The purity of all the tested compounds was greater than 95%, as determined by HPLC (Agilent 1100 Series).