Optical rotation measurements were made on a Rudolph research analytical AUTOPOL IV automatic polarimeter (Rudolph Research Analytical, Hackettstown, NJ, USA), IR spectra were recorded with a Bruker ALPHA II FT-IR spectrometer (Bruker, Billerica, MA, USA), and UV spectra were measured with a Thermo Scientific Nanodrop 2000C spectrophotometer (Thermo Fisher Scientific, Waltham, MA, USA). The ECD spectrum was obtained on a JASCO J-1500 circular dichroism spectrometer (Jasco, Easton, MD, USA). High-performance liquid chromatography (HPLC) was performed using a Varian ProStar 215 solvent delivery module equipped with a Varian ProStar 320 UV-Vis detector (Agilent Technologies, Santa Clara, CA, USA), operating under Star 6.41 chromatography workstation software (Agilent Technologies, Santa Clara, CA, USA). NMR spectra were obtained with a Bruker Avance III NMR spectrometer (Bruker, Billerica, MA, USA) equipped with a 3 mm cryogenic probe and operating at 600 MHz for 1H and 150 MHz for 13C. Spectra were calibrated to residual solvent signals at δH 2.50 and δC 39.5 in DMSO-d6. All 2D-NMR experiments were acquired with nonuniform sampling (NUS) set to 50% or 25%. HRESIMS data were acquired on an Agilent Technologies 6530 Accurate-Mass Q-TOF LC/MS instrument (Agilent Technologies, Santa Clara, CA, USA).
6530 accurate mass q tof lc ms instrument
Manufactured by Agilent Technologies
Sourced in United States
The 6530 Accurate-Mass Q-TOF LC/MS instrument is a high-performance liquid chromatography-mass spectrometry (LC-MS) system designed for accurate mass analysis. It features a quadrupole time-of-flight (Q-TOF) mass analyzer that provides precise mass measurements and high-resolution separation of complex samples.
Automatically generated - may contain errors
Lab products found in correlation
Avance 3 nmr spectrometer, by Bruker (1 mentions)
J 1500 circular dichroism spectrometer, by Jasco (1 mentions)
Thermo scientific nanodrop 2000c spectrophotometer, by Thermo Fisher Scientific (1 mentions)
Autopol 4 automatic polarimeter, by Rudolph Research Analytical (1 mentions)
Alpha 2 ft ir spectrometer, by Bruker (1 mentions)
Lc 20a series, by Shimadzu (1 mentions)
2 protocols using 6530 accurate mass q tof lc ms instrument
1
Comprehensive Analytical Characterization
2
Characterization of MOM-protected Acetophenones
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Solvents and reagents were supplied from Aldrich, Acros, or Fisher
and used without further purification. NMR spectra were recorded on
a Bruker AM-400 (400 MHz) spectrometer. High-resolution mass spectra
were obtained on an Agilent 6530 Accurate Mass Q-TOF LC/MS instrument.
Reactions in pressure tube were carried out using a Q-Tube reactor
from Q Labtech. Microwave reactions were conducted using a Biotage
Initiator reactor. All reactions were monitored by either TLC or HPLC.
Compounds were purified by flash chromatography on silica gel on a
Biotage Isolera One system. The purity of compounds was determined
by analytical HPLC (Shimadzu LC-20A series) using a Gemini, 3 μm,
C18, 110 Å column (50 mm × 4.6 mm, Phenomenex) and flow
rate of 1 mL/min. Gradient conditions were the following: solvent
A (0.1% trifluoroacetic acid in water) and solvent B (acetonitrile),
0–2.0 min 100% A, 2.0–7.0 min 0–100% B (linear
gradient), 7.0–8.0 min 100% B, UV detection at 254 and 220
nm. All the tested compounds were obtained with ≥95% purity
by HPLC. NMR standards used are as follows. 1H NMR: CDCl3, 7.26 ppm; CD3OD, 3.31 ppm; DMSO-d6, 2.50 ppm. 13C NMR: CDCl3, 77.16
ppm; CD3OD, 49.00 ppm; DMSO-d6, 39.52 ppm. MOM-protected acetophenones were synthesized as described
in the literature.56 (link),69 (link),70 (link)
and used without further purification. NMR spectra were recorded on
a Bruker AM-400 (400 MHz) spectrometer. High-resolution mass spectra
were obtained on an Agilent 6530 Accurate Mass Q-TOF LC/MS instrument.
Reactions in pressure tube were carried out using a Q-Tube reactor
from Q Labtech. Microwave reactions were conducted using a Biotage
Initiator reactor. All reactions were monitored by either TLC or HPLC.
Compounds were purified by flash chromatography on silica gel on a
Biotage Isolera One system. The purity of compounds was determined
by analytical HPLC (Shimadzu LC-20A series) using a Gemini, 3 μm,
C18, 110 Å column (50 mm × 4.6 mm, Phenomenex) and flow
rate of 1 mL/min. Gradient conditions were the following: solvent
A (0.1% trifluoroacetic acid in water) and solvent B (acetonitrile),
0–2.0 min 100% A, 2.0–7.0 min 0–100% B (linear
gradient), 7.0–8.0 min 100% B, UV detection at 254 and 220
nm. All the tested compounds were obtained with ≥95% purity
by HPLC. NMR standards used are as follows. 1H NMR: CDCl3, 7.26 ppm; CD3OD, 3.31 ppm; DMSO-d6, 2.50 ppm. 13C NMR: CDCl3, 77.16
ppm; CD3OD, 49.00 ppm; DMSO-d6, 39.52 ppm. MOM-protected acetophenones were synthesized as described
in the literature.56 (link),69 (link),70 (link)
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