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12 protocols using mercury 300

1

Spectroscopic Characterization of Organic Compounds

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The 1H NMR spectra were recorded in CDCl3, CD3OD or D2O on the following spectrometers: Varian Mercury-300 and Bruker Avance III (600 MHz) with TMS as an internal standard; chemical shifts δ in ppm with respect to TMS; coupling constants J in Hz. The 13C NMR spectra were recorded for CDCl3, CD3OD or D2O solutions on Varian Mercury-300 and Bruker Avance III (600 MHz) machines at 75.5 and 150.5 MHz, respectively. The 31P NMR spectra were recorded in CDCl3, CD3OD or D2O on Varian Mercury-300 and Bruker Avance III (600 MHz) spectrometers at 121.5 and 243 MHz, respectively.
IR spectra were measured on an Infinity MI-60 FT-IR spectrometer. Melting points were determined on the Boetius apparatus. Elemental analyses were performed by the microanalytical laboratory of the host institution on Perkin Elmer PE 2400 CHNS analyzer and the results were found to be in good agreement (±0.3 %) with the calculated values.
The following absorbents were used: column chromatography, Merck silica gel 60 (70–230 mesh); analytical TLC, Merck TLC plastic sheets, silica gel 60 F254. TLC plates were developed in chloroform–methanol solvent systems. Visualization of spots was effected with iodine vapours. All solvents were dried according to standard literature methods.
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2

Spectroscopic Characterization of Organic Compounds

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1H NMR were taken in CDCl3 or CD3OD on the following spectrometers: Varian Mercury-300 and Bruker Avance III (600 MHz) with TMS as an internal standard; chemical shifts δ in ppm with respect to TMS; coupling constants J in Hz. 13C NMR spectra were recorded for CDCl3,CD3OD or DMSO-d6 solutions on a Varian Mercury-300 and Bruker Avance III (600 MHz) spectrometer at 75.5 and 150.5 MHz, respectively. 31P NMR spectra were taken in CDCl3 or CD3OD on Varian Mercury-300 and Bruker Avance III at 121.5 and 242 MHz.
IR spectral data were measured on an Infinity MI-60 FT-IR spectrometer. Melting points were determined on a Boetius apparatus and are uncorrected. Elemental analyses were performed by the Microanalytical Laboratory of this Faculty on a Perkin Elmer PE 2400 CHNS analyzer. Polarimetric measurements were conducted on an Optical Activity PolAAr 3001 apparatus.
The following adsorbents were used: column chromatography, Merck silica gel 60 (70–230 mesh); analytical TLC, Merck TLC plastic sheets silica gel 60 F254. TLC plates were developed in chloroformmethanol solvent systems. Visualization of the spots was effected with iodine vapours. All solvents were purified by methods described in the literature.
All microwave irradiation experiments were carried out in a microwave reactor Plazmartonika RM 800. The reaction carried out in 50 mL-glass vials.
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3

NMR and Elemental Analysis Methods

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1H NMR spectra were taken in CDCl3 on the following spectrometers: Varian Mercury-300 and Bruker Avance III (600 MHz) with TMS as internal standard. 13C NMR spectra were recorded for CDCl3 solution on the Varian Mercur-300 machine at 75.5 MHz, while for DMSO solution on Bruker Avance III at 151.0 MHz. 31P NMR spectra were performed in CDCl3 solution on the Varian Mercury-300 at 121.5 MHz or on Bruker Avance III at 243.0 MHz. IR spectra were measured on an Infinity MI-60 FT-IR spectrometer. Melting points were determined on Boetius apparatus and are uncorrected. Elemental analyses were performed by the Microanalytical Laboratory of this Faculty on Perkin–Elmer PE 2400 CHNS analyzer. The following adsorbents were used: column chromatography, Merck silica gel 60 (70–230 mesh); analytical TLC, Merck TLC plastic sheets silica gel 60 F254.
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4

Spectroscopic Characterization of Compounds

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1H NMR spectra were taken in CDCl3, CD3OD and D2O on the following spectrometers: Varian Gemini 2000BB (200 MHz), Varian Mercury-300 and Bruker Avance III (600 MHz) with TMS as internal standard. 13C NMR spectra were recorded for CDCl3, CD3OD and D2O solution on the Bruker Avance III at 150 MHz and Varian Mercury-300 machine at 75 MHz. 31P NMR spectra were performed in CDCl3, CD3OD and D2O solution on the Varian Gemini 2000BB at 80.0 MHz, Varian Mercury-300 at 121 MHz or on Bruker Avance III at 242 MHz.
IR spectra were measured on an Infinity MI-60 FT-IR spectrometer. Melting points were determined on Boetius apparatus and are uncorrected. Elemental analyses were performed by the Microanalytical Laboratory of this Faculty on Perkin-Elmer PE 2400 CHNS analyzer.
The following adsorbents were used: column chromatography, Merck silica gel 60 (70–230 mesh); analytical TLC, Merck TLC plastic sheets silica gel 60 F254.
Preparative HPLC experiment was performed on a Waters apparatus equipped with Waters 2545 binary gradient module and Waters 2998 photodiode array detector (190–600 nm).
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5

Nuclear Magnetic Resonance Spectroscopy Protocol

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1H and 13C nuclear magnetic resonance (NMR) spectra
were recorded on Varian Gemini 300, Varian Mercury 300, Bruker ARX
300, Bruker DRX 400, Bruker AV 400, and Bruker AV-NEO 500 spectrometers
at 300, 400, or 500 MHz (1H) and 75 MHz, 100 MHz, or 125
MHz (13C), respectively. Chemical shifts (δ) are
reported in parts per million downfield from tetramethylsilane using
the residual deuterated solvent signals as an internal reference.
For 1H NMR, coupling constants J are given
in hertz, and the resonance multiplicity is described as s (singlet),
d (doublet), t (triplet), q (quartet), m (multiplet), and br (broad).
All spectra were recorded at 25 °C. Mass spectrometry (MS) and
high-resolution mass spectrometry (HR-MS) were performed by the MS-service
of the Laboratory for Organic Chemistry at the ETH Zürich on
a Waters Micromass AutoSpec-Ultima spectrometer (EI), on a Bruker
maXis spectrometer (ESI), or on a Varian IonSpec FT-ICR spectrometer
(MALDI). For MALDI measurements, the matrix was 2-[(2E)-3-(4-tert-butylphenyl)-2-methylprop-2-enylidene]malononitrile
(DCTB) or 3-hydroxypyridine-2-carboxylic acid (3-HPA). Masses are
reported in m/z units for the molecular
ion M+ for the exact
(ChemDraw) and the detected mass. NMR spectra can be obtained upon
request.
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6

Spectroscopic Analysis of Novel Compounds

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The NMR spectra were recorded at 300, 400, 500 (1H), and 75, 100, 125 (13C) MHz on a Varian Mercury 300, Bruker High-Performance Digital FT-NMR 400 Avance III, and JOEl ECA 500 MHz spectrometer, respectively, using a convenient solvent. The chemical shifts (δ) are reported in parts per million (ppm) and coupling constants (J) in Hz. Herein, Gallenkamp electrothermal melting point apparatus and electrothermal digital apparatus were used. EI-MS spectra were taken on HP; MS-5988. The UV analyses of the pure samples were recorded, separately, as MeOH solutions and with different diagnostic UV shift reagents on a Shimadzu UV 240 (P/N 240-5800) UV–visible spectrophotometer.
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7

Comprehensive Analytical Characterization

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1H NMR spectra
were recorded in CDCl3 on the following
spectrometers: Varian Mercury-300 and Bruker Avance III (600 MHz)
with tetramethylsilane as the internal standard. 13C NMR
spectra were recorded for CDCl3 solution on the Varian
Mercur-300 machine at 75.5 MHz, whereas for DMSO solution on Bruker
Avance III at 151.0 MHz. IR spectra were recorded on an Infinity MI-60
FT-IR spectrometer. Melting points were determined on Boetius apparatus
and were uncorrected. Elemental analyses were carried out on a PerkinElmer
PE 2400 CHNS analyzer. The following adsorbents were used: column
chromatography, Merck silica gel 60 (70–230 mesh); analytical
TLC, Merck TLC plastic sheets silica gel 60 F254.
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8

Synthesis and Polymerization of Compounds 3a-h

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The details of the synthesis and characterization of compounds 3a–h and their spontaneous polymerization are described in Supporting Information. The synthetic intermediates and the solvents were purchased from Sigma-Aldrich (Saint Louis, MO, USA) unless otherwise stated. NMR spectra were recorded with a Bruker (Karlsruhe, Germany) AC200, a Varian (Palo Alto, CA, USA) Mercury-300, a Bruker DRX-400 AVANCE, or a Bruker DRX-600 AVANCE spectrometer in the indicated solvents (TMS as internal standard). The values of the chemical shifts are expressed in ppm and the coupling constants (J) in Hz. An Agilent (Santa Clara, CA, USA) 1100 LC/MSD operating with an electrospray source was used in mass spectrometry experiments.
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9

Synthesis of Dendrimer G3Si(SC2H4NHFITC)(SC2H4CO2Na)31

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Dendrimer G3Si(SC2H4NHFITC)(SC2H4CO2Na)31 was synthesized following the protocol described in the bibliography with the appropriate modifications described [50 (link)]. The procedure is described below. Solvents and the chemicals were purchased from commercial sources and used without prior treatment. Thiol-ene reactions were carried out using a UV lamp that radiates vertically (high efficiency with VL-115.L Viber Lourmat filter, 365 nm emission, 30 W, 1100 µW/cm2). NMR experiments were performed on Varian spectrometers, Mercury-300 or Unity-500 spectrometers or Bruker AV400, at ambient temperature. The chemical shifts (ppm) were measured relative to the residual signal of 1H of the deuterated solvents. Infrared spectra were measured in the IR-FT Perkin-Elmer Spectrum 2000, and ultraviolet spectra were taken from the UV-Vis spectrophotometer Perkin-Elmer Lambda 35.
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10

Analytical Techniques for Organic Compounds

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Melting points were determined in open capillaries in a Gallenkamp apparatus, and are uncorrected. Merck silica gel 60 (230–400 mesh) was used for column chromatography. Merck TLC plates, silica gel 60 F254, were used for TLC. Bruker (Karlsruhe, Germany) AC200, a Varian Mercury-300 (Palo Alto, CA, USA), a Bruker DRX-400 AVANCE, or a Bruker DRX-600 AVANCE spectrometer in the indicated solvents (TMS as internal standard) were used to record the NMR spectra. In NMR spectra, the coupling constants (J) in Hz and the values of the chemical shifts are expressed in ppm. Mass spectrometry experiments were performed using an Agilent (Santa Clara, CA, USA) 1100 LC/MSD operating with an electrospray source.
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