All moisture-sensitive reactions were carried out in an oven dried flask under argon atmosphere. All chemicals and reagents were purchased from commercial suppliers and used without further purification. Anhydrous solvents were obtained as follows: anhydrous tetrahydrofuran, diethyl ether, and benzene were distilled from sodium metal under argon. Anhydrous dichloromethane, toluene, methanol, and acetonitrile were dried via distillation from CaH2 under argon. All other solvents were HPLC grade. 1H NMR and 13C NMR spectra were recorded on Varian INOVA300-1, Bruker Avance ARX-400 and Bruker DRX-500 spectrometers. NMR data are reported as: δ value (chemical shift, J-value (Hz), integration, where s=singlet, d=doublet, t=triplet, q=quartet, br= broad). Low resolution mass analyses were performed on a Agilent 1290 Infinity II spectrometer. High-resolution mass spectrometric analyses were performed at the Purdue University Campus-wide Mass Spectrometry Center. TLC analysis was carried out with SiliCycle 60A-F254 plates. Flash chromatography was performed using SiliCycle 230–400 mesh, 60 Å pore diameter silica gel. HPLC analysis was performed on a Agilent 1260 Infinity instrument. All test inhibitors showed purity >95% by HPLC analysis.
Avance arx 400
Manufactured by Bruker
Sourced in Japan
The Avance ARX-400 is a high-performance nuclear magnetic resonance (NMR) spectrometer designed for analytical and research applications in various fields, including chemistry, biochemistry, and materials science. It operates at a frequency of 400 MHz and provides reliable and accurate data acquisition and analysis capabilities.
Automatically generated - may contain errors
Lab products found in correlation
Inova300 1, by Bruker (2 mentions)
Agilent 1260 infinity instrument, by Agilent Technologies (1 mentions)
Drx 500, by Bruker (1 mentions)
Dip 370 polarimeter, by Jasco (1 mentions)
Uv 2075, by Jasco (1 mentions)
Pump module c 605, by Büchi (1 mentions)
Pump manager c 615, by Büchi (1 mentions)
Pu 2087, by Jasco (1 mentions)
Dg 2080 53, by Jasco (1 mentions)
Mx 2080 32, by Jasco (1 mentions)
α cyano 4 hydroxycinnamic acid, by Shimadzu (1 mentions)
341 polarimeter, by PerkinElmer (1 mentions)
1100 instrument, by Agilent Technologies (1 mentions)
Silica gel 60 f254 plate, by Merck Group (1 mentions)
Whatman, by Cytiva (1 mentions)
4 protocols using avance arx 400
1
Moisture-Sensitive Organic Synthesis Protocols
2
Chromatographic Analysis and Spectroscopic Characterization
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Thin layer chromatography (TLC) was conducted by using precoated silica gel 600 F254 plates (Art. 5715, Merck, Darmstadt, Germany) or reverse phase C18 F254 plates (Art. 15389, Merck, Darmstadt, Germany). Flash column chromatography was carried out on silica gel by a medium-pressure gradient system equipped with a Pump Module C-605 and a Pump Manager C-615 (BÜCHI, Flawil, Switzerland). High resolution ESIMS were recorded on a Mariner Biospectrometry Workstation (Applied Biosystems of Thermo Fisher Scientific, Waltham, MA, USA) equipped with an electrospray ion source in the positive mode. High performance liquid chromatography (HPLC) was performed on a high pressure gradient system that is composed of pumps PU-2087, a degasser DG-2080-53, a mixer MX-2080-32, and a detector UV-2075 (JASCO, Tokyo, Japan). FT-IR spectra were recorded on an FT/IR-400 spectrometer instrument (JASCO). Specific rotations were observed on a DIP-370 polarimeter (JASCO). NMR spectra were investigated on an Avance ARX400 (400 MHz for 1H) or Avance III HD 600 MHz Cryo-probe spectrometer (600 MHz for 1H) (Bruker Bio Spin, Yokohama, Japan). The chemical shifts (ppm) were referenced to the solvent residual peak at δH 7.26 ppm (CDCl3), δH 3.30/δC 49.0 ppm (CD3OD), or δH 2.06/δC 29.9 ppm (acetone-d6).
3
NMR and Mass Spectrometry Analysis
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NMR spectra were recorded on an Avance ARX400 (400 MHz for 1H) (Bruker Biospin, Yokohama, Japan). The chemical shifts (δ, ppm) were referenced to the internal standard (0.01% MeOH in D2O) at δH 3.334 and δC 49.5. MALDI-TOF MS was measured by a TOF/TOF 5800 spectrometer (AB Sciex, Foster, CA, USA) with α-cyano-4-hydroxycinnamic acid (Shimadzu Co., Tokyo, Japan) as a matrix. The calibration of MALDI-TOF MS was performed by using a mixture of PEG2000 and PEG4000 as an external calibrant. LC/MS was recorded on an HCTplus-ESI ion trap mass spectrometer (Bruker Daltonics Inc., Billerica, MA, USA) in the negative ion mode.
4
Anhydrous Synthesis with Detailed Spectroscopic Analysis
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