Chemical reagents were purchased from commercial sources (Sigma-Aldrich (St. Louis, MO, USA), Alfa Aesar (Ward Hill, MA, USA), Duksan Pure Chemicals, Daejung Chemicals, Samchun Pure Chemical, and Tokyo Chemical Industry) and used without further purification. 1H-NMR and 13C-NMR spectra were recorded on an NMR spectrometer (400 MHz, JEOL and Bruker). Mass spectra were obtained using a mass spectrometer (LTQ Orbitrap, Thermo Fisher Scientific, Waltham, MA, USA). The melting points of the materials were determined using melting point determination apparatus (M-565, Buchi, Meierseggstrasse 40, 9230 Flawil, Switzerland). Ultraviolet–visible (UV-vis) and fluorescence spectra, which were used for screening the materials, were recorded using UV-vis (V-630, JASCO Inc., Easton, MD, USA) and fluorescence spectrophotometers (Cary Eclipse, Agilent, Santa Clara, CA, USA), respectively. A pH meter (SevenCompact S210, Mettler Toledo, Greifensee, Switzerland) and a pH electrode (InLab Science Pro-ISM, Metter Toledo, Greifensee, Switzerland) were used to perform pH measurements.
M 565
Manufactured by Büchi
Sourced in Switzerland
The M-565 is a rotary evaporator designed for efficient solvent removal and concentration of liquid samples. It features a motorized lift, digital temperature control, and a built-in vacuum controller for precise operation. The M-565 is suitable for a wide range of laboratory applications that require controlled evaporation of solvents.
Automatically generated - may contain errors
Lab products found in correlation
Sevencompact s210, by Mettler Toledo (1 mentions)
Ltq orbitrap, by Thermo Fisher Scientific (1 mentions)
Cary eclipse, by Agilent Technologies (1 mentions)
V 630, by Jasco (1 mentions)
Diclofenac, by Tokyo Chemical Industry (1 mentions)
Smart apex ccd area detector diffractometer, by Bruker (1 mentions)
Avance 3 500 mhz spectrometer, by Bruker (1 mentions)
Q extractive orbitrap mass spectrometer, by Thermo Fisher Scientific (1 mentions)
Avance 3 hd 300, by Bruker (1 mentions)
Spectrum 100 ftir spectrometer, by PerkinElmer (1 mentions)
Tlc silica gel 60 f254, by Merck Group (1 mentions)
P 2000 polarimeter, by Jasco (1 mentions)
Ascend 400 mhz spectrometer, by Bruker (1 mentions)
V 530 spectrophotometer, by Jasco (1 mentions)
Silica gel 60, by Merck Group (1 mentions)
Jms s3000, by JEOL (1 mentions)
Nicolet is5 ftir spectrometer, by Thermo Fisher Scientific (1 mentions)
V 570, by Hitachi (1 mentions)
F 4500 spectrophotometer, by Hitachi (1 mentions)
Jms 700, by JEOL (1 mentions)
13 protocols using m 565
1
Characterization of Chemical Compounds
2
Synthesis and Characterization of Acridine Compounds
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All the chemical compounds were purchased from Sigma-Aldrich (St. Louis, MO, USA) (acridine, 6,9-diamino-2-ethoxyacridine-DL-lactate monohydrate) and Tokyo Chemical Industry TCI (diclofenac) and used without purification. Melting points were determined on a Büchi M-565 (Flawil, Switzerland) capillary apparatus and were uncorrected.
3
Preparation and Characterization of Organic Compounds
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All reactions were carried out under air atmosphere unless otherwise noted. All 1H and 13C NMR spectra were recorded on a Bruker AVANCE III 500 MHz spectrometer in deuterated solvents with tetramethylsilane (TMS) as internal standard. NMR multiplicities are abbreviated as follows: s = singlet, d = doublet, t = triplet, q = quartet, sept = septet, m = multiplet, br = broad signal. Chemical shifts are given in ppm and are referenced to SiMe4 (1H, 13C) and all spectra were obtained at 25 °C in the solvent indicated. Coupling constants J are given in Hz. GC analyses were performed on Agilent 6890 instrument with FID detector using an HP-5 capillary column (30 m × 0.32 mm (i.d.), 0.25 μ). High-resolution mass spectra were recorded in the EI mode on Agilent 6210 TOF mass spectrometry. Flash column chromatography was performed on neutral SiO2 (200–300 mesh) with ethyl acetate/petroleum as eluent. Melting points were determined on BÜCHI M-565 apparatus. X-ray crystallography were performed on a Bruker Smart Apex CCD area detector diffractometer using graphite-monochromated Mo Kα radiation (λ = 0.71073 Å). Details of the X-ray structure determinations and refinements are provided in Table 5 . According to the synthetic procedures in the literature, the organic compounds 1 , 2 , 3 , and 4 were prepared in good yield [69 (link),71 (link),75 (link)].
4
Characterization of Organic Compounds
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All chemicals and starting materials were obtained from Sigma-Aldrich (Toluca MEX, Mexico and St. Louis, MO, USA). Reactions were monitored by TLC on 0.2 mm percolated silica gel 60 F254 plates (Sigma-Aldrich) and visualized using irradiation with a UV lamp. Melting points were determined in a BUCHI (model M-565) melting point apparatus. According to IUPAC rules, compounds were named using the automatic name generator tool implemented in ChemDraw Professional 16.0.1.4 software (PerkinElmer, Waltham, MA, USA).
5
Synthesis of Moisture-Sensitive Compounds
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All reactions with moisture-sensitive reagents were carried out under an Ar atmosphere in anhydrous solvents, which were prepared using standard procedures. Commercially available reagents were used as received. Reaction monitoring was done by thin-layer chromatography (TLC) on precoated silica gel plates (Merck TLC Silica gel 60 F254). Spots were visualized by UV light (254 nm or 366 nm) or by staining with aqueous KMnO4, vanillin, or phosphomolybdic acid (PMA). Silica gel (40–63 μm) was used for column chromatography. Melting points were measured on a Büchi M-565 melting point apparatus and are uncorrected. Optical rotations were recorded through 5 continuous repetitions on a Jasco P-2000 polarimeter (1 dm cell) at 589 nm and concentrations close to 1.0% in chloroform or methanol. Infrared spectra were recorded on a PerkinElmer Spectrum 100 FT-IR spectrometer. NMR spectra were measured on Bruker Avance III HD 300 and 500 instruments and calibrated using the residual non-deuterated solvent as an internal reference. High resolution mass spectrometry (HRMS) was performed on a ThermoFischer Scientific Q-Extractive (Orbitrap) mass spectrometer using electrospray ionization (ESI). Compounds 12aa–ad were synthesized in 92–96% yield according to literature.27,28
6
Silica Gel-Based Chromatographic Techniques
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Silica gel (grade 60, 230-400 mesh) was used for column chromatography. Analytical HPTLC were performed on precoated plates of Silica gel 60, and the chromatograms were visualized by spraying the plates with 5% H 2 SO 4 /EtOH reagent followed by heating. Melting points (mp) were determined in a Büchi M-565 apparatus. Optical rotations were measured with an ADP 220 Bellenghan + Stanley Ltd. polarimeter at 25 • C. NMR analysis was performed on a Bruker 600 MHz Avance spectrometer and a Bruker/Avance DPX 250 MHz spectrometer.
7
Spectroscopic Characterization of Organic Compounds
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Melting points (°C, uncorrected) were measured on a BÜCHI M-565 melting point apparatus. IR spectral data were recorded on an ART FT-IR model ALPHA spectrophotometer, while UV spectra were generated via a JASCO V-530 spectrophotometer. HR-NMR data in CDCl3 (TMS as an internal reference) were obtained with a Bruker Ascend 400 MHz spectrometer. HR-ESI-MS data were measured using a Bruker LC/MS/MS QTOF model Maxis YHR-TOF mass spectrometer. Silica gel 60 (70–230 mesh, Merck, Kenilworth, NJ, USA) was used for column chromatography. Pre-coated TLC plates 60 F254 (20 × 20 cm, Merck) were used for analytical purposes, and the bands were visualized by UV light. Solvents for extraction and chromatography were distilled at their boiling point ranges prior to use but were analytical grade for recrystallization.
8
Characterization of Organic Compounds
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Melting points were measured on a Büchi M-565 apparatus and were uncorrected. NMR spectra were obtained with an AL-400 spectrometer at ambient temperature by using CDCl3 as a solvent and tetramethylsilane as an internal standard for 1H and 13C, unless otherwise indicated. IR spectra were obtained on a Thermo Scientific Nicolet iS5 FT-IR spectrometer with an iD5 ATR diamond plate. UV-vis-NIR and fluorescence spectra were recorded on Jasco V-570 and Hitachi F-4500 spectrophotometers, respectively. Absolute quantum yields were measured with a Hamamatsu Photonics C 9920-03G spectrophotometer. Mass spectra were obtained either with a JEOL JMS-700 (EI, 70 eV; FAB+, p-nitrobenzyl alcohol) or with a JEOL JMS-S3000 (MALDI-TOF). Elemental analyses were performed with a Yanaco MT-5 elemental analyzer at ADRES, Ehime University. Preparative GPC using LC-911 or LC-916 with Jaigel-1H and 2H was performed by Japan Analytical Industry Ltd. Co. Dehydrated solvents were purchased from Kanto Chemical Co. and used without further purification. Commercially available materials were used without further purification.
9
Detailed Organic Synthesis Characterization Protocol
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All chemical reagents were purchased from Merck (Darmstadt, Germany), Fluka (Darmstadt, Germany), or Sigma-Aldrich (St. Louis, MI, USA) and used without previous purification. All solvents were distilled and stored over proper desiccants. Melting points were measured on a BUCHI M-565 equipment. NMR spectra were recorded at 298 K on 400 NMR spectrometers, Varian Mercury (Varian, Palo Alto, CA, USA) and Avance Neo 400 Digital (Bruker, Rheinstetten, Germany), at 400 MHz and 101 MHz for 1H and 13C, respectively. All spectra were referenced using the TMS signal or the residual peak of the solvent. Chemical shifts (δ) are reported in ppm and coupling constants (J) are given in Hz. A TripleToF 6600-1 (Sciex, MA, USA) mass spectrometer was used for high-resolution mass spectrometry (HRMS). Silica gel (Merck, Darmstadt, Germany, 70–230 mesh) was used for column chromatography and Silica gel plates (Fluka, Darmstadt, Germany), and HF254 for thin-layer chromatography (TLC). TLC spots were detected by heating after staining with cerium molybdate in H2SO4. The cell viability analysis was conducted on a microplate spectrophotometer (OMEGA) at 570 nm. All abbreviation used are listed in Table S2 .
10
Spectroscopic and Thermal Analysis Protocol
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UV spectra of isolated
compounds were recorded on a Shimadzu UV–vis spectrophotometer
(UV2600, Japan). IR spectra were recorded on an Agilent FT-IR spectrometer
(Cary 660 series, USA). Melting points were measured on the Buchi
melting point apparatus (M-565, Buchi, Switzerland). 1H
NMR and 13C NMR were recorded on an Avance Neo 500 MHz
FT-NMR Spectrometer (Bruker, Switzerland) at 500 and 125 MHz, respectively.
Chemical shifts were recorded in δ (ppm) values relative to
tetramethylsilane as an internal reference. Thermogravimetric analysis
TGA analysis was done using a Perkin Elmer simultaneous thermal analyzer
(STA 8000, USA) in the temperature range of 30 to 800 °C. High-resolution
mass spectra (HR-MS) were recorded on Waters Micromass Q-Tof Micro,
USA. Trace metal analysis was done on ICP-MS Agilent 7800 series (USA)
using pure helium gas. XRD analysis was carried out on a Panalytical
X’PERT PRO X-ray diffractometer at scattering angle (2θ)
versus intensity, step size 0.001°, working voltage 45 kV with
a Cu Kα Ni-filtered radiation (λ = 1.5406 Å). Elemental
analysis was performed on an Elementar CHNOS Analyzer (Vario MACRO
cube, Germany).
compounds were recorded on a Shimadzu UV–vis spectrophotometer
(UV2600, Japan). IR spectra were recorded on an Agilent FT-IR spectrometer
(Cary 660 series, USA). Melting points were measured on the Buchi
melting point apparatus (M-565, Buchi, Switzerland). 1H
NMR and 13C NMR were recorded on an Avance Neo 500 MHz
FT-NMR Spectrometer (Bruker, Switzerland) at 500 and 125 MHz, respectively.
Chemical shifts were recorded in δ (ppm) values relative to
tetramethylsilane as an internal reference. Thermogravimetric analysis
TGA analysis was done using a Perkin Elmer simultaneous thermal analyzer
(STA 8000, USA) in the temperature range of 30 to 800 °C. High-resolution
mass spectra (HR-MS) were recorded on Waters Micromass Q-Tof Micro,
USA. Trace metal analysis was done on ICP-MS Agilent 7800 series (USA)
using pure helium gas. XRD analysis was carried out on a Panalytical
X’PERT PRO X-ray diffractometer at scattering angle (2θ)
versus intensity, step size 0.001°, working voltage 45 kV with
a Cu Kα Ni-filtered radiation (λ = 1.5406 Å). Elemental
analysis was performed on an Elementar CHNOS Analyzer (Vario MACRO
cube, Germany).
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