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6 protocols using mcp 300 polarimeter

1

Spectroscopic Characterization of Compounds

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The melting points were recorded on a SGW X-4B micro melting point apparatus (Shanghai Precision Scientific Instrument Co., Ltd, Shanghai, China) and were uncorrected. Optical rotations were determined using an MCP 300 polarimeter (Anton Paar, Graz, Austria) at 25 °C. UV data were recorded on a TU-1900 spectrophotometer (Persee, Beijing, China) in MeOH solution. ECD spectra were recorded using a Chirascan CD spectrometer (Applied Photophysics, London, UK). IR spectra were recorded on a Nicolet Nexus 670 spectrophotometer (Thermo Nicolet Corporation, Madison, WI, USA) in KBr discs. All NMR experiments were measured with Bruker Avance 500 spectrometers (500 and 125 MHz) (Bruker BioSpin, Switzerland), and the residual solvent peaks of CDCl3C 77.1/δH 7.26), acetone-d6C 29.8 and 206.3/δH 2.05), or methanol-d4C 49.0/δH 3.31) were used as references. HRESIMS data were acquired on a Thermo Fisher LTQ Orbitrap Elite high-resolution mass spectrometer (Thermo Fisher Scientific, Waltham, MA, USA). Column chromatography (CC) was carried by silica gel (200–300 mesh, Qingdao Maine Chemical Factory) and Sephadex LH-20 (GE Healthcare Bio-Sciences AB, Stockholm, Sweden). Semipreparative HPLC was performed on a Primaide HPLC system (Hitachi Instrument Dalian Co., Ltd, Dalian, China) with an Ultimate XB-C18 column (10 × 250 mm, 10 μm).
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2

Optical, UV, and NMR Characterization

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Optical rotations were measured at 20 °C in methanol using an Anton Paar MCP 300 polarimeter (Anton Paar, Graz, Austria) in a 100 mm long 350 μL cell. UV spectra for pure molecules were recorded at 20 °C in methanol using a PerkinElmer Lambda 5 spectrophotometer. NMR spectra were recorded on Bruker 500 MHz and 700 MHz spectrometers (Bruker, Rheinstetten, Germany). The chemical shifts (δ) are reported as ppm based on the solvent signal, and coupling constants (J) are in hertz. All solvents were HPLC grade, purchased from Sigma-Aldrich (Saint-Quentin-Fallavier, France).
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3

Optical, UV, and NMR Analysis of Compounds

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Optical rotations were measured at 20 °C in methanol using an Anton Paar MCP 300 polarimeter in a 100 mm long 350 μL cell (Anton Paar, Graz, Austria) . UV spectra were recorded at 20 °C in MeOH using a PerkinElmer Lambda 5 spectrophotometer (Thermo Fisher scientific, Les Ulis, France). NMR spectra were recorded on Bruker 700 MHz spectrometers (Bruker, Rheinstetten, Germany). The chemical shifts (δ) are reported as ppm based on the solvent signal, and the coupling constants (J) are given in hertz. Preparative HPLC was conducted with a Gilson system equipped with a 322 pumping device, a GX-271 fraction collector, a 171 diode array detector, and a prep ELSII. All solvents were HPLC grade and purchased from Sigma–Aldrich (Saint-Quentin-Fallavier, France).
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4

Spectroscopic Analysis of Organic Compounds

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Optical rotations were measured using an MCP-300 polarimeter (Anton Paar, Les Ulis, France). 1D and 2D NMR spectra were recorded on Avance 500 and 600 MHz spectrometers (Bruker, Wissembourg, France). The chemical shifts are relative to the residual signal solvent (CD3OD: δH 3.31; δC 49.20). High-resolution mass spectra were obtained on an LCT Premier XE spectrometer (Waters, Guyancourt, France) in electrospray ionization mode by direct infusion of the purified compounds. Chromatography on silica gel columns, was carried out on silica (Macherey-Nagel 60, 40–63 µm, Hoerdt, France), using a gradient of cyclohexane, ethyl acetate, methylene chloride, and methanol (Sigma-Aldrich, Saint-Quentin Fallavier, France). High performance liquid chromatography was performed on a 1260 Infinity system (Agilent, Les Ulis, France) equipped with a photodiode array detector (G1315C), an evaporative light scattering detector (G4260B), using an analytical reversed phase column Uptisphere C18 (4.6 mm × 250 mm, 5 µm, Interchim, Montluçon, France), and a semi-preparative Uptishere C18 (7.8 × 250 mm, 5 µm).
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5

Spectroscopic Characterization of Organic Compounds

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Optical rotations were measured using MCP-300 polarimeter (Anton Paar, Les Ulis, France). IR spectra were recorded on a BX FT-IR spectrometer (Perkin Elmer, Courtaboeuf, France). 1D and 2D NMR spectra were recorded on a Avance 500 and 600 MHz (CNRS-ICSN, Bruker, Wissembourg, France). The chemical shifts are relative to the residual signal solvent (CD3OD: δH 3.31; δC 49.20; DMF-d7: δH 8.03, 2.92, 2.75; δC 163.2, 34.9, 29.8). High-resolution mass spectra were obtained on a LCT Premier XE spectrometer (Waters, Guyancourt, France) in electrospray ionization mode by direct infusion of the purified compounds. Preparative HPLC was performed using Auto Prep system (Waters 600 controller and Waters 600 pump, equipped with a 996 Photodiode Array Detector, Waters, Guyancourt, France). A Varioskan® Flash microplate reader (Thermo Scientific, Villebon-sur-Yvette, France) was used for the acetylcholinesterase experiments.
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6

Comprehensive Analytical Techniques for Natural Products

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General Experimental Procedures. Optical rotations were measured using an Anton Paar MCP 300 polarimeter in a 350 µL cell with a length of 100 mm. UV spectra were recorded in acetonitrile using a PerkinElmer Lambda 5 spectrophotometer. Specific rotation was obtained in CHCl 3 with a JASCO P-1010 polarimeter. IR spectra were obtained on a Nicolet FTIR 205 spectrophotometer. Circular dichroism spectra were acquired on a Jasco® J-810 spectropolarimeter in a 1 cm cell at 20°C and treated with the SpectroManager® software.
NMR spectra were recorded in CD3OD or CD3CN on a Bruker 500 MHz spectrometer or a Bruker 600 MHz spectrometer equipped with a 2 mm invers detection probe. Chemical shifts (δ) are reported in ppm based on TMS signal. Coupling constants (J) are in hertz. High-Resolution ElectroSpray Ionization-TOF MS in positive mode (HRESI-TOF) measurements were performed using a Waters Acquity UPLC system with column bypass coupled to a Waters Micromass LCT Premier time-of-flight mass spectrometer equipped with an electrospray interface (ESI). All solvents were HPLC grade and HPLC-grade water was obtained with a Milli-Q water purification system (Synergy, Merck).
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