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8 protocols using jmn eca600

1

Spectroscopic Characterization of Compounds

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Optical rotations were measured on a JASCO P-2200 digital polarimeter. CD spectra were recorded on JASCO J-820 spectrometer. Infrared spectra (IR) were obtained with a Thermo Fisher Scientific NICOLET iS5 FT-TR spectrometer from samples in CH2Cl2. NMR spectra were measured on JEOL JMN-ECA600 and JMN-ECS400 spectrometers with tetramethylsilane as an internal standard, and chemical shifts are stated as δ values. HRMS data were recorded on a JMS-700 MStation quadrupole (FAB) or JMS-T100TD TOF (DART) mass spectrometer. A crystal of the compound was measured on a R-AXIS RAPID II (Rigaku). Analytical and preparative TLC were carried out on precoated silica gel 60F254 and RP-18F254 plates (0.25 or 0.50 mm thickness; Merck). MPLC was performed on Combiflash Rf (Teledyne Isco) with silica gel and C18 cartridges (Biotage, Uppsala Sweden). Preparative HPLC was operated on a GL Science recycling system using an InertSustain C18 column (5 μm, 20 × 250 mm).
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2

Analytical Methods for Compound Characterization

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Optical rotations were determined on a JASCO P-2200 digital polarimeter. ECD spectra were measured on a JASCO J-820 spectrometer. Infrared spectra (IR) were recorded with a Thermo Fisher Scientific NICOLET iS5 FT-TR spectrometer with samples in CH2Cl2. NMR spectra were obtained on JEOL JMN-ECA600 and JMN-ECS400 NMR spectrometers with tetramethylsilane as an internal standard, and chemical shifts are stated as δ values. HRMS data were recorded on a JMS-SX102A (FAB) or JMS-T100TD (DART) mass spectrometer. Analytical and preparative TLC were performed on precoated silica gel 60F254 and RP-18F254 plates (0.25 or 0.50 mm thickness; Merck). MPLC was performed on a Combiflash Rf (Teledyne Isco) instrument with silica gel and C18 cartridges (ODS-25, YMC-DispoPack). Preparative HPLC was conducted on a GL Science recycling system using an InertSustain C18 column (5 µM, 20 × 250 mm).
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3

Analytical Techniques for Chemical Structure Elucidation

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A JASCO P-2200 digital polarimeter was used for the determination of optical rotations. ECD spectra were detected on a JASCO J-820 spectrometer. NMR spectra were taken on JEOL JMN-ECA600 and JMN-ECS400 NMR spectrometers. Tetramethylsilane was used as an internal standard, and chemical shifts are stated as δ values. HRMS data were obtained on a JMS-SX102A (FAB) or JMS-T100TD (DART) mass spectrometer. Analytical and preparative TLC were conducted on RP-18F254 plates and precoated silica gel 60F254 (0.50 or 0.25 mm thickness; Merck). Column chromatography was performed with silica gel 60 N (63–210 μm, spherical, neutral, Kanto Chemical). Silica gel 60 RP-18 F254S (0.25 mm, Merck) was applied for reversed-phase and 60 F254 (1 mm) for normal-phase preparative TLC.
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4

Spectroscopic Characterization of Organic Compounds

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Optical rotations were recorded on a JASCO P-2200 digital polarimeter. Infrared spectra (IR) were measured with a Shimadzu FTIR-8700 instrument for samples in CHCl3. NMR spectra were taken on a JEOL JMN-ECA600 spectrometer and JMN-ECS400 spectrometer with tetramethylsilane as an internal standard, and chemical shifts are expressed as δ values. High-resolution mass spectrometric data were obtained on a JEOL JMS-700 (FAB) or a JMS-T100TD (DART) mass spectrometer. Analytical and preparative TLC was carried out on precoated silica gel 60F254 and RP-18F254 plates (0.25 or 0.50 mm thickness; Merck). MPLC was performed with silica gel and C18 cartridges (Biotage, Uppsala, Sweden).
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5

Characterization of Synthetic Compounds

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Optical rotations were recorded on a JASCO P-2200 digital polarimeter. Infrared spectra (IR) were measured with a Shimadzu FTIR-8700 instrument for samples in CHCl3. NMR spectra were acquired on JEOL JMN-ECA600 and JMN-ECS400 spectrometers with tetramethylsilane as internal standard, and chemical shifts are expressed as δ values. HRMS data were obtained on a JMS-SX102A (FAB) or JMS-T100TD (DART) mass spectrometer. Microwave irradiation experiments were carried out in a dedicated Biotage Initiator 2.5 microwave apparatus. Analytical and preparative TLC was carried out on precoated silica gel 60F254 and RP-18F254 plates (0.25 or 0.50 mm thickness; Merck). MPLC was performed with silica gel and C18 cartridges (Biotage, Uppsala Sweden). Compounds 91316 ,17 (link),20 and 1921 (link) were obtained previously.
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6

Characterization of Organic Compounds

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Optical rotations were recorded on a JASCO P-2200 digital polarimeter. Infrared spectra (IR) were measured with a Shimadzu FTIR-8700 instrument for samples in CHCl3. NMR spectra were recorded on JEOL JMN-ECA600 and JMN-ECS400 spectrometers with tetramethylsilane as an internal standard, and chemical shifts are expressed as δ values. HRMS data were obtained on a JMS-SX102A (FAB) or JMS-T100TD (DART) mass spectrometer. Analytical and preparative TLC were carried out on precoated silica gel 60F254 and RP-18F254 plates (0.25 or 0.50 mm thickness; Merck). MPLC was performed with silica gel and C18 cartridges (Biotage, Uppsala Sweden).
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7

Spectroscopic Characterization of Compounds

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Optical rotations were determined using a JASCO P-2200 digital polarimeter (JASCO, Tokyo, Japan). The UV spectra were measured with a Thermo Scientific Genesys 50 spectrometer (Thermo Scientific, Waltham, MA, USA). ECD spectra were measured with a JASCO J-820 spectrometer. Infrared spectra (IR) were recorded with a Shimadzu IRSpirit FT-IR spectrometer (Shimadzu, Kyoto, Japan) with a QATR-S single reflection ATR accessory, using neat samples. The NMR spectra were obtained via the JEOL JMN-ECA600 and JMN-ECS400 NMR spectrometers (JEOL, Akishima, Japan), with tetramethylsilane as an internal standard; chemical shifts are stated as δ values. HRMS data were recorded on a JMS-700 MStation (FAB) mass spectrometer. MPLC analysis was performed with C18 cartridges (Sfär C18 D, Biotage, Charlotte, NC, USA). Preparative HPLC analysis was conducted on a GL Science recycling system using an InertSustain C18 column (5 μm; 20 × 250 mm) (GL Sciences, Tokyo, Japan). LC/MS analysis was recorded with a Shimadzu LCMS-9030 connected to an Imtakt Cadenza CX-C18 (2 × 50 mm; 3 μm) (Imtakt, Kyoto, Japan).
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8

NMR Spectroscopy and Chromatography Protocol

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NMR spectra were measured on JEOL JMN-ECA600 and JMN-ECS400 spectrometers with tetramethylsilane as an internal standard and CDCl3 as solvent for both 1 H and 13 C NMR, and chemical shifts are stated as δ values. Analytical and preparative thin-layer chromatography (TLC) were performed using precoated silica gel 60 F254 plates (0.25 mm, Merck) for normal-phase and silica gel 60 RP-18 F254S plates (0.25 mm, Merck) for reversedphase. Column chromatography was carried out with silica gel 60 N (Spherical, 63-210 µm, neutral, Kanto Chemical).
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