For the stability of the compounds please see the Supplementary Material section. All chemicals were obtained from commercial sources and used without further purification. NMR spectra were obtained using a Bruker DPX 300 spectrometer (300 MHz, 1H NMR) or a Bruker AVANCE III 500 MHz with a TXI gradient probe. All spectra were referenced to residual solvent signal or TMS. HPLC was performed on a Waters system using a 1525EF pump and a 2489 UV detector. For preparative HPLC, a Dr. Maisch GmbH, Reprosil-Pur 120 C18-AQ 10 µm column and a gradient of 0.1 % TFA in H2O/CH3CN (95:5) to 0.1 % TFA in H2O/CH3CN (5:95) in 40 min were used. For analytical HPLC, a Dr. Maisch GmbH, Reprosil-Pur C18-AQ 5 μm (250×4.6 mm) column and a gradient of 0.1 % TFA in H2O/CH3CN (95:5) to 0.1 % TFA in H2O/CH3CN (5:95) in 40 min were used. MALDI-ToF measurements were performed on a Bruker Microflex. High-resolution mass spectra were measured on an Exactive orbitrap high-resolution mass spectrometer (Thermo Fisher Scientific, San Jose, CA) and processed with the use of Thermo Scientific Xcalibur software (V2.1.0.1139). For dialysis, Sigma Pur-A-LyzerTM Mega 3,500 units were used.
1525ef pump
Manufactured by Waters Corporation
Sourced in Netherlands
The 1525EF pump is a high-performance liquid chromatography (HPLC) pump designed for use in analytical laboratories. It offers precise and reliable solvent delivery for a variety of HPLC applications.
Automatically generated - may contain errors
Lab products found in correlation
Reprosil pur c18 aq 5 μm 250 4.6 mm column, by Dr. Maisch (2 mentions)
Avance 3 500 mhz, by Bruker (1 mentions)
Dpx 300 spectrometer, by Bruker (1 mentions)
Xcalibur software, by Thermo Fisher Scientific (1 mentions)
Microflex, by Bruker (1 mentions)
Avance 3 500, by Bruker (1 mentions)
Uv 2401pc, by Shimadzu (1 mentions)
Fraction collector 3, by Waters Corporation (1 mentions)
Avance 3 600, by Bruker (1 mentions)
2998 photodiode array detector, by Waters Corporation (1 mentions)
Uplc it tof, by Shimadzu (1 mentions)
Uv 2700, by Shimadzu (1 mentions)
Hplc system, by Waters Corporation (1 mentions)
Microflex lrf maldi tof, by Bruker (1 mentions)
3 protocols using 1525ef pump
1
Analytical Characterization of Compounds
2
Analytical Techniques for Compound Characterization
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UV spectra were recorded on Shimadzu UV-2700 and UV-2401PC spectrometers. Optical rotations were measured with an automatic polarimeter RUDOLPH APVI-6. 1D and 2D NMR spectra were obtained on Bruker AVANCE III-500 and AVANCE III-600 MHz spectrometers with SiMe4 as internal standard. MS data were obtained using Shimadzu UPLC-IT-TOF (Shimadzu Corp, Kyoto, Japan). Column chromatography (CC) was performed on silica gel (200–300 mesh, Qing-dao Haiyang Chemical Co., Ltd., Qingdao, China) or RP-18 silica gel (20–45 µm, Fuji Silysia Chemical Ltd., Japan). Fractions were examined by TLC on silica gel plates (GF254, Qingdao Haiyang Chemical Co., Ltd., Qingdao, China) and spots are visualized with Dragendorff’s spray reagent. MPLC was performed using a Buchi pump system in combination with glass columns filled with RP-18 silica gel (19 × 480, 40 × 480, 45 × 480 and 55 × 480 mm, respectively). HPLC analysis was performed using a Waters 1525 EF pump in combination with a Sunfire C18 pre- or semi-preparative analysis column (4.6 × 150 and 19 × 250 mm, respectively) The HPLC system is combined with a Waters 2998 Photodiode Array Detector and Waters Fraction Collector III [22 (link)].
3
Purification and Analysis of Organic Compounds
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All chemicals were obtained
from commercial
sources and used without further purification. Solvents were obtained
from Actu-All Chemicals (Oss, The Netherlands) in HPLC grade and used
without further purification. The reactions were monitored by thin-layer
chromatography (TLC) and mass spectrometry using a Bruker microflex
LRF MALDI-TOF. HPLC was performed on a Waters (Etten-Leur, The Netherlands)
HPLC system using a 1525EF pump and a 2489 UV/vis detector. For preparative
HPLC, a Dr Maisch GmbH (Ammerbuch, Germany) Reprosil-Pur 120 C18-AQ
10 μm (250 × 20 mm) column was used (12 mL/min). For analytical
HPLC, a Dr Maisch GmbH Reprosil-Pur C18-AQ 5 μm (250 ×
4.6 mm) column was used, applying a gradient of 0.1% TFA in H2O/CH3CN 95:5 to 0.1% TFA in H2O/CH3CN 5:95 in 40 min (1 mL/min).
from commercial
sources and used without further purification. Solvents were obtained
from Actu-All Chemicals (Oss, The Netherlands) in HPLC grade and used
without further purification. The reactions were monitored by thin-layer
chromatography (TLC) and mass spectrometry using a Bruker microflex
LRF MALDI-TOF. HPLC was performed on a Waters (Etten-Leur, The Netherlands)
HPLC system using a 1525EF pump and a 2489 UV/vis detector. For preparative
HPLC, a Dr Maisch GmbH (Ammerbuch, Germany) Reprosil-Pur 120 C18-AQ
10 μm (250 × 20 mm) column was used (12 mL/min). For analytical
HPLC, a Dr Maisch GmbH Reprosil-Pur C18-AQ 5 μm (250 ×
4.6 mm) column was used, applying a gradient of 0.1% TFA in H2O/CH3CN 95:5 to 0.1% TFA in H2O/CH3CN 5:95 in 40 min (1 mL/min).
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