The reactions were performed under an air atmosphere unless otherwise stated. All solvents and reagents were employed as received. Analytical thin layer chromatography (TLC) was performed on SiO2 60 F254 plates and flash column chromatography was carried out using SiO2 60 (particle size 0.040–0.055 mm, 230–400 mesh), both of which are available from E. Merck (Darmstadt, Germany). Visualization was performed under UV irradiation at 254 nm followed by staining with aqueous potassium permanganate [KMnO4 (3 g) and K2CO3 (20 g) in 300 mL of H2O containing 5 mL of an aqueous solution of NaOH (5%, w/v)] and charring by heat gun. 1H- and 13C-NMR spectra were recorded on a 500 FT NMR instrument (Bruker, Billerica, MA, USA). Chloroform-d and methanol-d were used as solvents and TMS (δ = 0.00 ppm) as an internal standard. Chemical shifts are reported as δ values in ppm as referenced to TMS. Multiplicities are recorded as s (singlet), d (doublet), t (triplet), q (quartet), quint (quintet), sext (sextet), sept (septet), dd (doublet of doublets), dt (doublet of triplets), br (broad), m (multiplet). Coupling constants (J) are expressed in Hz. LRMS and HRMS were measured by a JMS-HX110 spectrometer (JEOL, Tokyo, Japan) and spectroscopic data were recorded as m/z values. Melting points were measured using an Electrothermal instrument (Anatec Yanaco Inc., Kyoto, Japan).
Sio2 60
Manufactured by Merck Group
Sourced in Germany
SiO2 60 is a type of laboratory equipment used for chromatography applications. It is a silica gel-based material designed for the separation and purification of various chemical compounds. The product provides a high surface area and pore volume to facilitate efficient separation and purification processes. No further details on intended use or applications are provided.
Automatically generated - may contain errors
Lab products found in correlation
Model 241 polarimeter, by PerkinElmer (1 mentions)
Unity inova, by Agilent Technologies (1 mentions)
Silica gel 60 f254, by Merck Group (1 mentions)
Acquity column, by Waters Corporation (1 mentions)
Jms hx110 spectrometer, by JEOL (1 mentions)
Gemini 500, by Agilent Technologies (1 mentions)
Gemini 300, by Agilent Technologies (1 mentions)
Sephadex lh 20, by GE Healthcare (1 mentions)
6 protocols using sio2 60
1
General Analytical Procedures for Organic Synthesis
2
Spectroscopic Analysis of Organic Compounds
3
Structural Characterization of Compounds
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IR spectra were obtained using KBr disks or films on a Perkin–Elmer FT 1605 spectrophotometer. NMR spectra including COrrelation SpectroscopY (COSY), Nuclear Overhauser Effect SpectroscopY (NOESY), Heteronuclear Multiple Bond Correlation (HMBC) and Heteronuclear Single Quantum Correlation (HSQC) experiments were acquired on a Varian Unity INOVA at 300 or 400 MHz (1H) and 75 or 100 MHz (13C). Electron impact mass spectrometry (EI-MS) was recorded on a JEOL SX 102A mass spectrometer and optical rotations were determined on a Perkin–Elmer Model 241 polarimeter. For open column chromatography, SiO2 60 (70–230 mesh, Merck, Germany) was used and silica gel 60 F254 (Merck) for TLC.
4
C109 Metabolite Identification in B. cenocepacia
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To identify the products of C109 transformation in the cellular environment, 200 ml B. cenocepacia J2315 culture were grown overnight at 37°C in LB medium, then 20 mg C109 were added. After 1.5 h, a chloroform extraction (100 ml × 3) was performed. Organic phase obtained from the extraction was evaporated, residues were resuspended in hexane/ethyl acetate 9:1 and subjected to flash column chromatography (Merck SiO2 60, 230–400 mesh). Visualization of metabolites was achieved under UV light at a wavelength of 254 nm.
The isolated metabolites were analyzed in UPLC/MS. The chromatographic analysis was performed with a JASCO X-LC (Lecco, Italy) system, coupled with a Thermo Fisher Scientific (Milan, Italy) LTQ XL HESI-MS/MS system. Chromatography was performed on a Waters Acquity column, 3 um particle size, 0.3 ml/min, gradient 10 min from 90:10 H2O/MeCN to 100% MeCN, then 4 min in 100% MeCN. The analyses were performed in full-scan from 150 and 2,000 u.m.a. in positive mode, and base peaks were analyzed with dependent scan method with @CID = 32 eV. Run were also monitored by recording the absorbance at 220 nm.
The isolated metabolites were analyzed in UPLC/MS. The chromatographic analysis was performed with a JASCO X-LC (Lecco, Italy) system, coupled with a Thermo Fisher Scientific (Milan, Italy) LTQ XL HESI-MS/MS system. Chromatography was performed on a Waters Acquity column, 3 um particle size, 0.3 ml/min, gradient 10 min from 90:10 H2O/MeCN to 100% MeCN, then 4 min in 100% MeCN. The analyses were performed in full-scan from 150 and 2,000 u.m.a. in positive mode, and base peaks were analyzed with dependent scan method with @CID = 32 eV. Run were also monitored by recording the absorbance at 220 nm.
5
Isolation of Compounds from C. macrolepis var. formosana
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The dried bark of C. macrolepis var. formosana (16 kg) was extracted with acetone (140 L) at room temperature (two times, 7 days/each time). The acetone extract (1.8 kg) was suspended in H2O, then partitioned with EtOAc. The EtOAc layer (734 g)was subjected to open column chromatography (SiO2 60, 70–230 mesh; Merck), and purified by repeated normal-phase HPLC with mixtures of n-hexane and EtOAc as eluents. Compounds 2 (H/E = 6:4, 2.4 mg), 3 (H/E = 6:4, 1.5mg), 4a (H/E = 7:3, 2.1mg), 5 (H/E = 4:1, 1.5mg), 6 (H/E = 4:1, 1.9mg), 7 (H/E = 7:3, 2.0mg), 8 (H/E = 9:1, 2.2mg), 9 (H/E= 4:1, 1.3mg), 10 (H/E=7:3, 4.5mg), 11 (H/E = 4:1, 9.3 mg), 12 (H/E = 6:4, 6.3 mg), and 13 (H/E = 9:1, 10.2 mg) were obtained using above solvent systems as mobile phase, respectively.
6
Analytical Characterization of Natural Products
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All solvents (analytical and high performance liquid chromatography (HPLC) grade) were purchased from Vetec (Rio de Janeiro, Brazil), Quimex (São Paulo, Brazil), Qhemis (São Paulo, Brazil), Sigma-Aldrich (São Paulo, Brazil) and Tedia (Rio de Janeiro, Brazil) and used without further purification. Thin and preparative layer chromatography (TLC and PLC) were performed on glass plates covered with SiO 2 PF 254 Merck 60 and revealed with Dragendorff reagent, iodine vapor and/ or UV light at 254 and 365 nm. All chromatographic separations were performed on SiO 2 60 (70 -230 mesh) from Merck, Sephadex LH-20 (GE Healthcare) and functionalized octadecyl (200 -400 mesh) from Sigma-Aldrich. The sizes of the chromatographic columns used were 40 9 4.5 cm, 45 9 5 cm and 15 9 8 cm. IR Spectra: Bomem infrared spectrometer mark, MB100; ṽ in cm À1 . 1 H-and 13 C-(single and twodimensional) nuclear magnetic resonance (NMR) spectra were obtained on Varian spectrometers mark, Gemini-500 ( 1 H: 500 MHz and 13 C: 125 MHz); MR-400 ( 1 H: 400 MHz and 13 C: 100 MHz) and Gemini-300 ( 1 H: 300 MHz and 13 C: 75 MHz) using CDCl 3 , CD 3 OD and
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