Specific rotations were measured using a DIP-360 digital polarimeter (JASCO, Easton, PA, USA). Nuclear magnetic resonance (NMR) spectra were recorded on a JEOL ECX 400 FT-NMR spectrometer (JEOL, Tokyo, Japan) at room temperature. Electrospray ionization time-of-flight mass spectrometry (ESI-TOF-MS) experiments were performed using a Waters Xevo G2-XS Q-TOF mass spectrometer (Waters, Milford, MA, USA). Column chromatography was performed on Silica Gel 60 (Nacalai Tesque, Kyoto, Japan, 230–400 mesh) and YMC ODS-A gel (YMC Co. Ltd., Kyoto, Japan, 50 µm). Thin-layer chromatography (TLC) was performed on TLC Silica Gel 60F254 (Merck, Damstadt, Germany) and TLC Silica Gel 60 RP-18 F254S (Merck, Damstadt, Germany) plates. The spots were visualized by spraying with 10% aq. sulfuric acid followed by heating. High-performance liquid chromatography (HPLC) was performed using a UV-8020 UV-VIS detector (Tosoh Corp., Tokyo, Japan), DP-8020 pump (Tosoh Corp., Tokyo, Japan), and DP-8020 degasser (Tosoh Corp., Tokyo, Japan). An XBridge BEH C18 Column (Waters, Milford, MA, USA, 130 Å, 3.5 µm, 10 mm × 250 mm) was used for preparative purposes.
Dip 360 digital polarimeter
Manufactured by Jasco
Sourced in United States, Japan
The DIP-360 digital polarimeter is a laboratory instrument used to measure the rotation of polarized light passing through a sample. It accurately determines the optical rotation angle of a substance, which can provide information about its molecular structure and composition.
Automatically generated - may contain errors
Lab products found in correlation
4100 fourier transform infrared spectrophotometer, by Jasco (2 mentions)
Jnm eca500, by JEOL (2 mentions)
Xbridge beh c18 column, by Waters Corporation (1 mentions)
Silica gel 60, by Nacalai Tesque (1 mentions)
Gel ods a, by YMC (1 mentions)
Tlc silica gel 60 rp 18 f254s, by Merck Group (1 mentions)
Xevo g2 xs qtof mass spectrometer, by Waters Corporation (1 mentions)
Tlc silica gel 60 f254, by Merck Group (1 mentions)
Dp 8020 pump, by Tosoh (1 mentions)
Silica gel 60 f254, by Merck Group (1 mentions)
Jnm ecp 400 spectrometer, by JEOL (1 mentions)
Apex 2 diffractometer, by Bruker (1 mentions)
Apex3, by Bruker (1 mentions)
Uv 240 spectrophotometer, by Shimadzu (1 mentions)
Avance 3 600 ascend, by Bruker (1 mentions)
Hx 110 mass spectrometer, by JEOL (1 mentions)
6 protocols using dip 360 digital polarimeter
1
Analytical Methods for Structural Characterization
2
Synthetic Procedures for Chiral Compounds
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All reagents and dry solvents were purchased from commercial vendors and used directly without further purification. All reactions were placed in dried sample vials inserted with magnetic beads. Thin-layer chromatography (TLC) was performed on Merck silica gel 60 F254 plates and the analytes were identified under UV light. Flash column chromatography was performed using silica gel pore size 60N (40–100 μm). Melting points were recorded with a micro-melting point apparatus. IR spectra were recorded with a JASCO-4100 Fourier transform infrared spectrophotometer. 1H and 13C NMR spectroscopic data were recorded using a JEOL JNM-ECA500 instrument with tetramethyl silane as the internal standard. HPLC data were collected using the TOSOH instrument equipped with (UV-8020, DP-8020, and SD-8022) detectors using CHIRALPAK IB column. Optical rotations were recorded using a JASCO DIP-360 digital polarimeter. High-resolution mass spectrometry (HRMS) data were collected by electron impact (EI) modes using Hitachi RMG-GMG and JEOL JNX-DX303 sector instruments.
3
Microwave-Assisted Spectroscopic Analysis
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The microwave-assisted heating was carried out using a Green Motif-I apparatus (IDX Co, Ltd., Sano, Japan; single mode; output power 30–300 W) at 2.45 GHz [9 (link)]. The 1H and 13C NMR (400 MHz and 100 MHz, respectively) spectra were measured using a JNM-ECP400 spectrometer (JEOL Ltd., Tokyo, Japan) in D2O or CDCl3 with DSS or Me4Si as the internal standard (δ = 0 ppm). Optical rotations were measured by a DIP-360 digital polarimeter (JASCO Corporation, Tokyo, Japan). Melting points were determined using a 500-D micromelting point apparatus (Yanaco Analytical Systems Inc., Kyoto, Japan) and were uncorrected. High-resolution mass spectra (HRMS/ESI) data were obtained by a Thermo Scientific Exactive (Thermo Fisher Scientific K. K., Tokyo, Japan). Elemental analysis was conducted using a JM10 CHN Analyzer MICRO CORDER (J-Science Lab Co., Ltd., Kyoto, Japan). The high-performance liquid chromatography (HPLC) was performed using a Gilson HPLC system (Gilson Incorporated, Wisconsin, WI, USA) with a Shodex KS-801 column [80 °C, H2O, 0.5 mL/min] and SEDEX 55 ELSD detector.
4
Structural Elucidation of (-)-Mycousnine Enamine
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13C, 1H, and two-dimensional nuclear magnetic resonance (2D-NMR) as well as distortionless enhancement by polarization transfer (DEPT) spectrum were recorded on a BrukerDRX500 spectrometer using TMS as an internal standard. Coupling constants were recorded as J in Hertz and chemical shifts as δ values (parts per million). Melting points (MP) were detected on a Beijing X4 micro-melting point instrument. High-resolution mass spectra (HRESIMS) were tested on an Apex III Fourier-transforming ion cyclotron resonance (FTICR) Bruker mass spectrometer. Optical rotations ([α]20 D) were tested using a JASCO DIP-360 digital polarimeter. Single-crystal X-ray diffraction data were measured using a Bruker APEX2 diffractometer with graphite-monochromated Cu K radiation = 1.54178 Å. The crystallographic data for (-)mycousnine enamine in this paper have been deposited in the Cambridge Crystallographic Data Centre (CCDC) as supplementary publication number CCDC 1512383.
5
Synthesis and Characterization of Oxoindoline Derivatives
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All reagents and solvents used
in this work were bought from commercial channels and used directly.
Oxoindolines1a –m were prepared according
to the literature procedure.10 (link) All reactions
were placed under argon atmosphere in flame-dried 4 mL sample vials
inserted with magnetic beads. Thin-layer chromatography (TLC) was
performed on Merck silica gel 60 F254 plates, and the analytes
were identified under UV light. Flash column chromatography was performed
using silica gel pore size 60N (40–100 μm). Melting points
were recorded with a micro-melting-point apparatus. IR spectra were
recorded with a JASCO 4100 Fourier transform infrared spectrophotometer. 1H and 13C NMR spectroscopic data were recorded
using JEOL JNM-ECA500 instrument with tetramethylsilane as the internal
standard. X-ray diffraction data of4e were collected
at 93 K on a Rigaku R-AXIS RAPID diffractometer using multilayer mirror
monochromated Cu Kα radiation. HPLC data were collected using
TOSOH instrument equipped with (UV-8020, DP-8020, and SD-8022) detectors
using CHIRALCEL OD-H and CHIRALPAK AD-H columns. Optical rotations
were recorded using a JASCO DIP-360 digital polarimeter. High-resolution
mass spectrometry (HRMS) data were collected by electron impact (EI)
and fast atom bombardment (FAB) modes using Hitachi RMG-GMG and JEOL
JNX-DX303 sector instruments.
in this work were bought from commercial channels and used directly.
Oxoindolines
to the literature procedure.10 (link) All reactions
were placed under argon atmosphere in flame-dried 4 mL sample vials
inserted with magnetic beads. Thin-layer chromatography (TLC) was
performed on Merck silica gel 60 F254 plates, and the analytes
were identified under UV light. Flash column chromatography was performed
using silica gel pore size 60N (40–100 μm). Melting points
were recorded with a micro-melting-point apparatus. IR spectra were
recorded with a JASCO 4100 Fourier transform infrared spectrophotometer. 1H and 13C NMR spectroscopic data were recorded
using JEOL JNM-ECA500 instrument with tetramethylsilane as the internal
standard. X-ray diffraction data of
at 93 K on a Rigaku R-AXIS RAPID diffractometer using multilayer mirror
monochromated Cu Kα radiation. HPLC data were collected using
TOSOH instrument equipped with (UV-8020, DP-8020, and SD-8022) detectors
using CHIRALCEL OD-H and CHIRALPAK AD-H columns. Optical rotations
were recorded using a JASCO DIP-360 digital polarimeter. High-resolution
mass spectrometry (HRMS) data were collected by electron impact (EI)
and fast atom bombardment (FAB) modes using Hitachi RMG-GMG and JEOL
JNX-DX303 sector instruments.
6
Spectroscopic Characterization of Organic Compounds
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Melting points were determined on a Yanaco MP-S3 apparatus. UV spectra were measured on a Shimadzu UV 240 spectrophotometer. A JASCO DIP–360 Digital polarimeter was used to measure the optical rotations in chloroform by using a 10-cm cell tube. The 1H-NMR and 2D NMR spectra were recorded on a Bruker Avance III 600 Ascend spectrometer using the BBO probe, while 13C-NMR spectra were recorded on a Bruker Avance III 600 Ascend spectrometer operating at 125 MHz using CDCl3 as a solvent. Chemical shifts were reported in δ (ppm), relative to SiMe4 as internal standard, and coupling constants (J) were measured in Hz. The EI-MS and HREIMS were measured on the Jeol HX 110 mass spectrometer. Thin-layer chromatography (TLC) was performed on silica gel pre-coated plates (PF254 20 × 20, 0.25mm, Merck, Germany). Ceric sulfate in 10% H2SO4 spraying reagent was used for the staining of compounds on TLC. All reagents used were of analytical grades.
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