High resolution mass spectra were measured on Bruker micrOTOF II instruments using electrospray ionization (ESI HRMS) using standart published conditions [24 (link)].
Silica gel 60 f254 aluminum backed plates
Silica Gel 60 F254 aluminum-backed plates are a type of thin-layer chromatography (TLC) media. They consist of a thin layer of silica gel coated on an aluminum backing. The silica gel layer contains a fluorescent indicator (F254) that allows for the visualization of separated compounds under ultraviolet (UV) light.
2 protocols using silica gel 60 f254 aluminum backed plates
Organic Synthesis Techniques and Instrumentation
Synthesis and Characterization of Azobenzene Compounds
from commercial sources (Sigma-Aldrich, TCI Europe N.V., Strem Chemicals,
etc.) and were used without further purification. Solvents were obtained
from Fisher Scientific. Reactions were monitored by thin layer chromatography
(TLC) on precoated, Merck Silica gel 60 F254 aluminum-backed
plates, and the chromatograms were first visualized by UV irradiation
at λ = 254 nm. Flash silica gel chromatography was performed
using silica gel (SiO2, particle size 40–63 μm)
purchased from SiliCycle. NMR spectra were measured on a BRUKER Avance
III HD 400 (equipped with a CryoProbe). Multiplicities in the following
experimental procedures are abbreviated as follows: s = singlet, d
= doublet, t = triplet, q = quartet, m = multiplet. 1H
chemical shifts are expressed in parts per million (ppm, δ scale)
and are referenced to the residual protium in the NMR solvent (CDCl3: δ = 7.26; THF-d8: δ
= 1.72). 13C chemical shifts are expressed in ppm (δ
scale) and are referenced to the carbon resonance of the NMR solvent
(CDCl3: δ = 77.16, THF-d8: δ = 25.31). NOTE: Due to the trans/cis isomerization of some compounds containing an azobenzene
functionality, more signals were observed in the 1H and 13C spectra than would be expected for the pure trans-isomer. Only signals for the major trans-isomer
are reported.
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