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Mr 400 mhz

Manufactured by Agilent Technologies
Sourced in United States

The MR-400 MHz is a nuclear magnetic resonance (NMR) spectrometer designed for high-resolution analysis. It operates at a frequency of 400 MHz and is capable of performing advanced NMR spectroscopy techniques for the identification and structural elucidation of organic and inorganic compounds.

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3 protocols using mr 400 mhz

1

Synthesis and Characterization of CPTEG:SA Copolymer

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A 10:90 CPTEG:SA copolymer was synthesized as described previously [41 (link)]. Briefly, the diacids were acetylated at 140 °C for 30 min, and then reacted at 180 °C at 0.2 torr for 30–60 min, dissolved into methylene chloride (Thermo Fisher Scientific, Waltham, MA, USA), precipitated into hexanes (Thermo Fisher Scientific), and dried. The molecular weight of the copolymer was ~15,000 g/mol, as confirmed by proton nuclear magnetic resonance (NMR; MR-400 MHz, Varian, Palo Alto, CA, USA) spectroscopy.
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2

Characterization of Sunitinib Analogues

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All reagents from commercial sources were used without further purification unless otherwise noted. 1H-NMR spectra were taken in DMSO-d6, MeOD or CDCl3 at room temperature on Varian MR 400 MHz, Varian Vnmrs 500 MHz, and Varian Vnmrs 700 MHz instruments. The reported chemical shifts for the 1HNMR spectra were recorded in parts per million (ppm) on the δ scale from an internal tetramethylsilane standard (0.0 ppm). Small molecule mass spectrometry data was measured using a Waters Corporation Micromass LCT or Agilent6230 Q-TOF instrument. HPLC was used to determine purity of compounds on an Agilent 1100 series with an Agilent Zorbax Eclipse Plus-C18 column. A gradient of 10–90% acetonitrile/water over 6 minutes followed by 90% acetonitrile/water for 7 minutes was used with detection at 254 nm. Purity of all compounds was > 95% as determined by HPLC. The Sunitinib scaffold is well known to photoisomerize in solution17 (link), and thus our compounds represent a 70:30 mix of active versus inactive isomers. All figures in the paper depict the active isomer.
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3

Characterization of TFMOx Enantiomers

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An RS-mixture and samples of pure S-or R-TFMOx enantiomers were commercially obtained (SynQuest Laboratories) and used as received. Their chemical identity and purity were verified by nuclear magnetic resonance (NMR) spectroscopy. The 1 H, 13 C, and 19 F NMR data were recorded on Varian VNMRS-500 MHz or MR-400 MHz spectrometers at room temperature. Chemical shifts were referenced to residual protic impurities in the solvent ( 1 H) or the deuterio solvent itself ( 13 C) and reported relative to external Si(CH 3 ) 4
( 1 H, 13 C) or C 6 H 5 CF 3 ( 19 F). The chemical purity after integration of the fluorine NMR signal has been estimated to be higher than 96% for the RS-TFMOx mixture and higher than 96% or 98% for the S-TFMOx or R-TFMOx enantiomers, respectively. The NMR shifts were assigned based on 2D-NMR (HSQC) spectra. The enantiomeric purity of the samples was investigated by high-performance liquid chromatography (HPLC) using a CHIRALPAK IG (4.6 mm × 250 mm) chiral analytical column. According to these measurements, the RS-TFMOx mixture is racemic within margins of error (S-TFMOx : R-TFMOX = 49% : 51%), and the enantiopure S-TFMOx or R-TFMOx have an enantiomeric excess of approximately 95% (see Fig. 2 for details).
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