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2 protocols using ac 500 nmr spectrometer

1

Spectroscopic Characterization of Compounds

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1H-, 13C-NMR, DEPT and 2D-NMR spectra were recorded on a Bruker AC 500 NMR spectrometer with tetramethylsilane (TMS) as an internal standard. HR-ESI-MS data were measured on a Bruker microTOF-QII mass spectrometer. CD spectra were measured with a Chirascan circular dichroism spectrometer (Applied Photophysics, Surrey, UK). Optical rotation values were measured with a PerkineElmer 341 polarimeter. Column chromatography was performed on silica gel (200–300 mesh; Qingdao Marine Chemical Factory, Qingdao, China), YMC gel (ODS-A, 12 nm, S-50 µm) and Sephadex LH-20 (Amersham Biosciences, Uppsala, Sweden), respectively. The silica gel GF254 used for TLC were supplied by the Qingdao Marine Chemical Factory, Qingdao, China. All solvents used were of analytical grade (Tianjin Fuyu Chemical and Industry Factory, Tianjin, China). HPLC was carried on Hitachi L-2400 with YMC ODS column. Spots were detected on TLC under UV light or by heating after spraying with 5% H2SO4 in EtOH (v/v).
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2

Purification and Characterization of Organic Compounds

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CH3CN and CH2Cl2 were dried over CaH2 and stored over 4
Å molecular sieves, while pyridine and Et3N were dried
over KOH and stored over KOH. The progress of reactions was monitored
by TLC (pre-coated silica gel GF254 sheets (Merck 5554)). TLCs were
run in petroleum ether/EtOAc or CH2Cl2/MeOH
systems and were visualized with UV light and iodine spray and/or
by spraying perchloric acid solution and heating. Column chromatographic
separations were performed using silica gel 60–120 mesh (Merck)
or 200–400 mesh (Merck).
1H and 13C NMR spectra were recorded on a Bruker AC-200, AC-400, or AC-500
NMR spectrometer. The chemical shifts are referred to internal TMS
for 1H and chloroform-d for 13C NMR. Mass spectra were recorded on a Q Exactive Hybrid Quadrupole
Orbitrap Mass spectrometer (Thermo Fisher Scientific), MALDI-TOF spectra
were recorded on a SCIEX TOF/TOF 5800 system, and the matrix used
for analysis was THAP (2,4,6-trihydroxyacetophenone)/ammonium citrate
(2:1). UV experiments were carried out on a Varian Cary 300 UV-Visible
spectrophotometer equipped with a Peltier-controlled cell holder.
CD spectra were recorded on a Jasco J-815 spectropolarimeter equipped
with a Peltier-controlled cell holder.
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