Optical rotation was measured using a JASCO DIP-180 digital spectropolarimeter. IR spectra were recorded using a Nicolet 510P FT-IR spectrometer. UV spectra were measured in MeOH using a Shimadzu UV-1601PC spectrophotometer. The NMR spectra were recorded in CDCl3 at room temperature on a Varian Mercury plus 400 NMR spectrometer with residual solvent resonance as an internal reference. The 2D NMR spectra were recorded using the standard pulse sequences. For EI-MS and HR-EI-MS, Finnigan TSQ-700 and JEOL SX-102A spectrometers were used, respectively. TLC was performed on silica gel 60 F254 plates (Merck, Darmstadt, Germany). Column chromatography was performed on silica gel (230 400 mesh ASTM, Merck). HPLC was performed using a Hitachi L-7000 chromatograph with a Bischoff RI detector (Leonberg, Germany). A normal phase column (LiChrosorb Si 60, 7 μm, 250 × 10 mm, Merck) was used for isolation.
230 400 mesh astm
Manufactured by Merck Group
Sourced in Germany, Japan
230–400 mesh ASTM is a specification that defines the particle size range of a powdered material. It is a widely used standard in the laboratory equipment industry. This specification indicates that the material has a particle size distribution where 230 mesh corresponds to the minimum particle size and 400 mesh corresponds to the maximum particle size, as defined by the American Society for Testing and Materials (ASTM).
Automatically generated - may contain errors
Lab products found in correlation
Silica gel 60 f254 plate, by Merck Group (1 mentions)
Uv 1601 pc spectrophotometer, by Shimadzu (1 mentions)
Dip 180, by Jasco (1 mentions)
Mercury plus 400 nmr spectrometer, by Agilent Technologies (1 mentions)
Sx 102a, by JEOL (1 mentions)
Lichrosorb si 60, by Merck Group (1 mentions)
Kieselgel 60 f254 plate, by Merck Group (1 mentions)
Micromass quattro micro api, by Waters Corporation (1 mentions)
Jnm ecz500r, by JEOL (1 mentions)
Acquity uplc beh c18 column, by Waters Corporation (1 mentions)
Acquity uplc system, by Waters Corporation (1 mentions)
Spectrum 400 ft ir spectrometer, by PerkinElmer (1 mentions)
Eca 400 mhz nmr spectrometer, by JEOL (1 mentions)
1650 pc uv vis spectrophotometer, by Shimadzu (1 mentions)
Q tof micro, by Waters Corporation (1 mentions)
Mercury plus, by Agilent Technologies (1 mentions)
Drx 400 spectrometer, by Bruker (1 mentions)
Rp 18 f254, by Merck Group (1 mentions)
Sars cov 2 3clpro, by Merck Group (1 mentions)
Tlc silica gel 60 f254, by Merck Group (1 mentions)
6 protocols using 230 400 mesh astm
1
Comprehensive Spectroscopic Analysis of Compounds
2
Analytical Characterization of Organic Compounds
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Open column chromatography was performed using silica gel (230–400 mesh ASTM, Merck, Darmstadt, Germany), and thin-layer chromatography analysis was performed on Kieselgel 60 F254 plates (silica gel, Merck, Darmstadt, Germany). The compound was visualized under UV light (254 and 365 nm) and 20% (v/v) H2SO4 reagent (Duksan, Gyeonggi-do, Korea). NMR spectra were obtained using a JNM-ECZ500R (JEOL, Tokyo, Japan) with deuterium solvent (Cambridge Isotope Laboratories, Tewksbury, MA, USA) as an internal standard, and chemical shifts were expressed as δ values. The LC–ESI–MS experiment was performed using Waters Acquity UPLC system and Waters Micromass Quattro Micro API (Waters, Milford, MA, USA) with Acquity UPLC BEH C18 column (2.1 × 50 mm i.d. 1.7 μm, Waters, Milford, MA, USA).
3
Chromatographic Purification and Analysis
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Column chromatography was performed using silica gel 60, 230–400 mesh ASTM (Merck, 0.040–0.063mm). Aluminium supported silica gel 60 F254 plates 20 x 20cm (absorbent thickness: 0.25 mm) were used for thin layer chromatography (TLC) (Merck, Germany). Preparative thin layer chromatography (PTLC) (Merck, Germany) silica gel 60 F254 glass plates 20 x 20cm (absorbent thickness: 0.50 mm) were used for separation of compounds. IR spectrum was recorded using a Perkin-Elmer Spectrum 400 FT-IR Spectrometer with spectroscopic grade chloroform as the solvent. 1D- and 2D-NMR spectra were recorded in chloroform CDCl3 (Merck, Germany) using JEOL ECA 400 MHz NMR spectrometer. The LCMS-IT-TOF spectra were recorded on a UFLC Shimadzu Liquid Chromatography with a SPD-M20A diode array detector coupled to a IT-TOF mass spectrometer. UV spectra were recorded using a Shimadzu 1650 PC UV-Vis Spectrophotometer with spectroscopic grade methanol (CH3OH) as solvent. All solvents were of analytical grade and were distilled prior to use.
4
Chromatography and Spectroscopic Analysis
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Chromatography was performed on silica gel Merck 230–400 mesh ASTM. All melting points were determined using a Microquimica model MQAPF-301 apparatus. The high-resolution electron spray ionization mass spectrometry (HRESIMS) analyses were performed on a QTOF Micro (Waters, Manchester, UK) mass spectrometer equipped with an ESI source. Proton nuclear magnetic resonance (1H NMR) spectra were recorded using CDCl3 as a solvent at ambient temperature using a Varian Mercury Plus (300 MHz) with TMS as an internal standard. The chemical shifts (δ) are given in parts per million relative to TMS. Carbon-13 nuclear magnetic resonance (13C NMR) spectra were recorded at 75.5 MHz with the same internal standard.
5
NMR and TLC Analysis of SARS-CoV-2 3CLpro
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NMR experiments were conducted with a Bruker DRX-400 spectrometer (Bruker, Germany), with the chemical shift referenced to the residual solvent signals and using DMSO‑d6 as solvent. Thin-layer chromatography (TLC) analysis was performed on silica-gel 60 F254 and RP-18 F254S plates (both 0.25 mm layer thickness; Merck, Darmstadt, Germany). Compounds were visualized by dipping plates into 10 % (v/v) H2SO4 reagent, which were then air heat-treated at 300 °C for 15 s. Silica gel (60 A, 70–230 or 230–400 mesh ASTM; Merck) and reversed-phase silica gel (ODS-A 12 nm S-150, S-75 μm; YMC Co., Kyoto, Japan) were used for open column chromatography. SARS-CoV-2 3CLpro was purchased from Sigma Aldrich (St. Louis, MO, USA). DABCY-LKTSAVLQSGFRKME-EDANS was synthesized by Anygen (Gwangju, Korea).
6
Characterization of Organic Compounds
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General Information All the commercially available chemicals were obtained from Aldrich, Sigma, Fluka, and Junsei Chemical Company and used generally without further purification. Solvents including ethyl acetate and n-hexane for column chromatography were of technical grade and distilled before use.
The 1 H-NMR spectra (300 MHz 1 H) were recorded on Bruker Fourier Transform AG-300 and Varian Fourier Transform-300 instrument in chroroform-d 3 (CDCl 3 ) or dimethyl sulfoxide-d 6 (DMSO-d 6 ). Chemical shifts were reported in δ units (ppm), using tetramethylsilane (TMS) as internal standard. The following abbreviations were used to describe peak patterns when appropriate: s, singlet; d, doublet; t, triplet; q, quartet; m, multiplet. Coupling constant (J) was reported in Hertz unit (Hz). Mass spectra were recorded on a Varian 1200 L GC/MS using electron impact (EI) method.
All reactions were monitored using thin layer chromatography (TLC) on silica gel glass plates (E.Merck, TLC silica gel 60F 254 ). Visualization on TLC was achieved by UV light (254 nm), typical TLC indicating solution (p-anisaldehyde), iodine and polymolybdic acid indicator. Flash column chromatography was carried out using Merck 230-400 mesh ASTM.
The 1 H-NMR spectra (300 MHz 1 H) were recorded on Bruker Fourier Transform AG-300 and Varian Fourier Transform-300 instrument in chroroform-d 3 (CDCl 3 ) or dimethyl sulfoxide-d 6 (DMSO-d 6 ). Chemical shifts were reported in δ units (ppm), using tetramethylsilane (TMS) as internal standard. The following abbreviations were used to describe peak patterns when appropriate: s, singlet; d, doublet; t, triplet; q, quartet; m, multiplet. Coupling constant (J) was reported in Hertz unit (Hz). Mass spectra were recorded on a Varian 1200 L GC/MS using electron impact (EI) method.
All reactions were monitored using thin layer chromatography (TLC) on silica gel glass plates (E.Merck, TLC silica gel 60F 254 ). Visualization on TLC was achieved by UV light (254 nm), typical TLC indicating solution (p-anisaldehyde), iodine and polymolybdic acid indicator. Flash column chromatography was carried out using Merck 230-400 mesh ASTM.
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