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Avance 300

Manufactured by JEOL

The Avance 300 is a nuclear magnetic resonance (NMR) spectrometer manufactured by JEOL. It is designed to perform high-resolution NMR analysis of chemical and biological samples. The Avance 300 provides accurate measurements of molecular structure and dynamics.

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2 protocols using avance 300

1

NMR Spectroscopy, Mass Spectrometry, and X-Ray Crystallography Protocols

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1H and 13C NMR spectra were recorded on Bruker Avance 300, Jeol ECA 500, and Varian Inova 500 spectrometers. NMR multiplicities are abbreviated as follows: s = singlet, d = doublet, t = triplet, q = quartet, sept = septet, m = multiplet, br = broad signal. Chemical shifts are given in parts per million (ppm) and are referenced to SiMe4 (1H, 13C) and CFCl3 (19F). All spectra were obtained at 25°C in the solvent indicated. Coupling constants J are given in hertz (Hz). Mass spectra were performed at the University of California San Diego Mass Spectrometry Laboratory. Melting points were measured with an electrothermal MEL-TEMP apparatus. Single crystal x-ray diffraction data were collected on a Bruker Apex II CCD (charge-coupled device) detector using Mo-Kα radiation (λ = 0.71073 Å). Crystals were selected under oil, mounted on nylon loops, and then immediately placed in a cold stream of nitrogen. Structures were solved and refined using Olex2 and SHELXTL. The CAAC and 3,3-diphenyl-1-propyne were prepared following literature procedures, whereas all other starting materials were purchased from commercial sources.
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2

Purification and Characterization of Organic Compounds

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Chemicals purchased from commercial sources were used without further purification. All solvents were purified by distillation, dried according to standard procedures or were purchased in HPLC-quality. Preparative (flash) column chromatography was performed on Acros Silica gel 60 (0.035–0.070 mm, 60 Å) as stationary phase. All products were dried in high vacuum (10-3 bar). Thin layer chromatography (TLC) was performed on precoated aluminium silica gel SIL G/UV254 plates (Macherey-Nagel & Co., Düren, NRW, Germany). 1H-NMR (13C-NMR) spectra were recorded at room temperature on a Bruker Avance 300 or 400 or JEOL JNM GX 400 spectrometer. All chemical shifts are given in ppm scale and refer to the non-deuterized proportion of the solvent. NMR raw data was processed with the program MestReNova. Maldi Mass spectra were recorded with Shimadzu Biotech AXIMA Confidence. ESI Mass spectra were recorded with a Bruker Daltonik maXis 4G, a Bruker Daltonik micrOTOF II focus or an Agilent 6120 Quadrupole LCMS System. HPLC spectra were recorded at room temperature on an Agilent Technologies 1200 Series HPLC system. As a stationary phase, the following columns were utilized: IA, IB, IC, AS, OD. IR spectra were recorded on a Varian IR-660 apparatus. The Absorption is indicated in wave numbers (cm−1). Optical rotations were determined on a PerkinElmer polarimeter, model 341, λ = 546 nm.
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