All starting materials were commercially procured and were used without further purification, unless specified. Reaction solvents were purified by passage through alumina columns on a purification system manufactured by Innovative Technology (Newburyport, MA). For all microwave reactions a Biotage® Initiator+ was used and the absorbance was set in accordance with the recommendations set by the manufacturer. NMR spectra were obtained on Varian NMR systems, operating at 400 or 500 MHz for 1 H acquisitions. LCMS analysis was performed using a Waters Alliance reverse phase HPLC (columns Waters SunFire C18 4.6 × 50 mm, 3.5 μm, or Waters SunFire C8 4.6 × 50 mm, 3.5 μm), with single-wavelength UV–visible detector and LCT Premier time-of-flight mass spectrometer (electrospray ionization) or Waters Micromass ZQ detector (electrospray ionization). Optical rotations were obtained on a Jasco P-2000. Purification of intermediates and final compounds was performed using silica gel chromatography on a Biotage® Isolera™ One Flash purification system. Where required, final compounds were purified by preparative reverse phase HPLC (columns Waters Symmetry RP8 30 × 50 mm, 5 μm column, or OBD RP18 30 × 50 mm, 5 μm), with a single wavelength UV–visible detector and Waters Micromass ZQ (electrospray ionization). All final compounds have purities greater than 95% based upon LC/MS analysis.
Micromass zq detector
Manufactured by Waters Corporation
Sourced in United States
The Micromass ZQ detector is a mass spectrometry instrument designed to provide high-performance detection capabilities. It is capable of detecting and analyzing a wide range of molecular compounds with precision and accuracy.
Automatically generated - may contain errors
Lab products found in correlation
Sunfire c18, by Waters Corporation (2 mentions)
Nmr system, by Agilent Technologies (2 mentions)
Alliance reverse phase hplc, by Waters Corporation (2 mentions)
Sunfire c8, by Waters Corporation (2 mentions)
Isolera one flash purification system, by Biotage (2 mentions)
Waters micromass zq, by Waters Corporation (1 mentions)
Initiator, by Biotage (1 mentions)
P 2000, by Jasco (1 mentions)
Unity 400, by Agilent Technologies (1 mentions)
Fractionlynx system, by Waters Corporation (1 mentions)
4 protocols using micromass zq detector
1
Purification and Characterization of Compounds
2
Synthesis and characterization of novel compounds
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All reagents and solvents were purchased from commercial suppliers and used without further purification. Melting points were determined using Electrothermal 9001 analyzer and are uncorrected. 1H NMR spectra were recorded at 400 MHz on Varian Unity + 400. Shifts for NMR are reported in ppm downfield from TMS (s). A Waters Micromass ZQ detector was used in ESI MS for identification of various products. Elemental analyses were carried out using a C,H,F,N elemental analyzer, model Carlo-Erba 5500 instrument. The results are within ± 0.3% of the theoretical values. Merck silica gel 60 F254 plates were used for analytical TLC; column chromatography was performed on Merck silica gel 60 (70–230 mesh).
3
Purification and Characterization of Organic Compounds
4
Enantioseparation of d- and l-eflornithine
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The analytical SFC runs were
performed on an Acquity UPC2 instrument equipped with a
photodiode array detector and a single quadrupole detector using the
software Empower (version 3, Waters, Milford, MA, USA). The flow rate
was 3.5 mL/min, the back pressure was set to 120 bar, and the column
temperature was 40 °C. The preparative SFC system used was Supersep
150 equipped with a UV spectroscopy detector using the software Proficy
HMI/SCADA iFIX (version 5.1, Novasep, Pompey, France).
The analytical
HPLC runs were performed on Alliance 2695 equipped with a Waters Micromass
ZQ detector (Waters, Milford, USA) using the software MassLynx (version
4.1). The flow rate was 1 mL/min, and the initial column temperature
was 25 °C. The semipreparative HPLC system used was an Interchim
puriFlash 4250 integrated with a puriFlash AS-I sampler, UV, ELS,
and MS detectors using the software Interchim soft (V5.1c.09, Montluçon,
Cedex, France). The collectedd - and l -eflornithine
fractions were evaporated using a Rotavapor R II rotary evaporator
(BÜCHI Labortechnik AG, Flawil, Switzerland) and a Biotage
V-10 evaporator system (Biotage AB, Uppsala, Sweden). To identify
the elution order of the enantiomers, Chirobiotic TAG (4.6 ×
250 mm, 5 μm) with a mobile phase of buffer:EtOH 75:25 (v/v%)
(buffer containing 17 mM AcOH and 2 mM TEA) was used.33 (link)
performed on an Acquity UPC2 instrument equipped with a
photodiode array detector and a single quadrupole detector using the
software Empower (version 3, Waters, Milford, MA, USA). The flow rate
was 3.5 mL/min, the back pressure was set to 120 bar, and the column
temperature was 40 °C. The preparative SFC system used was Supersep
150 equipped with a UV spectroscopy detector using the software Proficy
HMI/SCADA iFIX (version 5.1, Novasep, Pompey, France).
The analytical
HPLC runs were performed on Alliance 2695 equipped with a Waters Micromass
ZQ detector (Waters, Milford, USA) using the software MassLynx (version
4.1). The flow rate was 1 mL/min, and the initial column temperature
was 25 °C. The semipreparative HPLC system used was an Interchim
puriFlash 4250 integrated with a puriFlash AS-I sampler, UV, ELS,
and MS detectors using the software Interchim soft (V5.1c.09, Montluçon,
Cedex, France). The collected
fractions were evaporated using a Rotavapor R II rotary evaporator
(BÜCHI Labortechnik AG, Flawil, Switzerland) and a Biotage
V-10 evaporator system (Biotage AB, Uppsala, Sweden). To identify
the elution order of the enantiomers, Chirobiotic TAG (4.6 ×
250 mm, 5 μm) with a mobile phase of buffer:EtOH 75:25 (v/v%)
(buffer containing 17 mM AcOH and 2 mM TEA) was used.33 (link)
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