All experimental manipulations were performed under purified dry nitrogen using standard Schlenk and vacuum line techniques. Solvents were dried and freshly distilled under an atmosphere of nitrogen prior to use [26 ]. The chemicals Mo(CO)6, W(CO)6, Cr(CO)6, chlorodiphenylphosphine, and p-aminoacetophenone were purchased from Aldrich and used as received. N-(4-acetylphenyl)-N-(diphenylphosphino)amine ligand (1 ) was previously prepared [19 ]. Infra-red spectra were recorded with a PerkinElmer System 2000 FT-IR spectrometer between 4000 and 400 cm−1 using KBr disks. Microanalyses were performed on a Flash 2000 elemental analyzer. Infra-red spectra were recorded on a Shimadzu FTIR-8400S spectrometer between 4000-400 cm−1 using KBr disks. The NMR spectra were recorded at 25 °C on a Bruker-Avance-DRX-400 MHz NMR spectrometer operating at 400.17 (1H), 100.63 (13C), and 161.98 (31P) using tetramethylsilane for 1H and 85% H3PO4 for 31P NMR as external standards. Melting points were carried out on a Gallenkamp apparatus with open capillaries.
Avance drx 400 mhz nmr spectrometer
Manufactured by Bruker
Sourced in United States
The Avance-DRX-400 MHz NMR spectrometer is a laboratory instrument designed for nuclear magnetic resonance (NMR) spectroscopy. It operates at a frequency of 400 MHz and is used for the analysis and characterization of chemical compounds.
Automatically generated - may contain errors
Lab products found in correlation
System 2000 ftir spectrometer, by PerkinElmer (1 mentions)
Ftir 8400s spectrometer, by Shimadzu (1 mentions)
W co 6, by Merck Group (1 mentions)
Mo co 6, by Merck Group (1 mentions)
Cr co 6, by Merck Group (1 mentions)
Dip 370 digital polarimeter, by Jasco (1 mentions)
Cary 630 ftir, by Agilent Technologies (1 mentions)
Topspin 3, by Bruker (1 mentions)
Solvent purification system, by MBraun (1 mentions)
Tensor 27 ir spectrometer, by Bruker (1 mentions)
3 protocols using avance drx 400 mhz nmr spectrometer
1
Synthesis and Characterization of Phosphino-Amine Complexes
2
Detailed NMR and Optical Characterization
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We performed 1D and 2D nuclear magnetic resonance (1H and 13C NMR, HSQC, and HMBC) spectroscopy employing a Brucker Avance III 500 MHz spectrometer equipped with a 5 mm TXI field gradient probe-head having dedicated channels for 1H, 13C, and 15N. Samples were prepared in deuterated chloroform (CDCl3) and results were analyzed with Bruker TopSpin 3.5 software. Some measurements were made with a Bruker Avance DRX 400 MHz NMR spectrometer equipped with various probe-heads and TopSpin version 2.1 software (Bruker BioSpin, Billerica, MA, USA).
Optical rotation data were collected using a Rudolph Research Analytical Autopol IV Automatic polarimeter (Hackettstown, NJ, USA) or Jasco DIP-370 Digital Polarimeter (Hachioji, Tokio, Japan). IR spectra were measured using a Thermo Scientific Nicolet iS10 FTIR spectrophotometer fitted with a Smart iTR (Waltham, MA, USA) or an Agilent Cary 630 FTIR controlled by MicroLab PC software (Santa Clara, CA, USA).
Optical rotation data were collected using a Rudolph Research Analytical Autopol IV Automatic polarimeter (Hackettstown, NJ, USA) or Jasco DIP-370 Digital Polarimeter (Hachioji, Tokio, Japan). IR spectra were measured using a Thermo Scientific Nicolet iS10 FTIR spectrophotometer fitted with a Smart iTR (Waltham, MA, USA) or an Agilent Cary 630 FTIR controlled by MicroLab PC software (Santa Clara, CA, USA).
3
Rhodium-Catalyzed Hydroboration Reactions
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All reactions and manipulations were carried out under a nitrogen atmosphere by using standard Schlenk techniques unless stated otherwise. Solvents were either obtained from an MBraun Solvent Purification System, or dried and stored according to common procedures. 11 Dimethylamine-borane is commercially available and was used as obtained. [{RhCl-(cod)} 2 ] and ligands VIIIa and VIIIb were synthesised according to literature procedures. 3g,12 NMR spectra were recorded with a Bruker AVANCE DRX 400 MHz NMR spectrometer at room temperature. All isolated compounds were measured in deuterated tetrahydrofuran (THF-d 8 ). Tetramethylsilane was used as internal standard for 1 H NMR spectra. 85% H 3 PO 4 was used as external standard for 31 P{ 1 H} NMR spectra, and BF 3 •OEt 2 was used as external standard for 11 B{ 1 H} NMR spectra. NMR spectra were recorded at the following frequencies: 1 H: 400.13 MHz, 11 B: 128.38 MHz, 31 P: 161.99 MHz. IR spectra were recorded as ATR spectra in the range of 4000-640 cm -1 with a Bruker TENSOR 27 IR spectrometer.
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