UV spectra were obtained with a Hitachi UV-3210 and UV-3010 spectrophotometer (Hitachi, Tokyo, Japan), and IR spectra were measured with a Shimadzu FTIR Prestige-21 spectrometer (Shimadzu, Kyoto, Japan). Optical rotations were measured with a HORIBA SEPA-300 digital polarimeter in a 0.5 dm cell (Horiba, Kyoto, Japan). The ESIMS and HRESIMS were taken on a Bruker Daltonics APEX II 30e spectrometer (Bruker, Billerica, MA, USA). 1H- and 13C-NMR spectra were measured using Bruker Avance-300, AMX-400, and AV-500 spectrometers (Bruker, Billerica, MA, USA) with TMS as the internal reference, and chemical shifts are expressed in δ (ppm). Silica gel (70–230 and 230–400 mesh; Merck, Darmstadt, Germany) and Spherical C18 100 Å reversed phase Silica gel (RP-18; particle size 20–40 μm; Silicycle, Quebec City, QC, Canada) were used for column chromatography (CC), and Silica gel 60 F254 and RP-18 F254S thin-layer chromatography (TLC) plates (Merck, Darmstadt, Germany) were used for preparative TLC, respectively.
Sepa 300 digital polarimeter
Manufactured by Horiba
Sourced in Japan
The SEPA-300 is a digital polarimeter manufactured by HORIBA. It is designed to measure the optical rotation of a sample, which is a property of certain substances that can be used to determine their chemical composition or concentration. The SEPA-300 provides accurate and reliable measurements of optical rotation angles.
Automatically generated - may contain errors
Lab products found in correlation
Apex 2 30e spectrometer, by Bruker (1 mentions)
Uv 3010 spectrophotometer, by Hitachi (1 mentions)
Ft ir prestige 21 spectrometer, by Shimadzu (1 mentions)
Amx 400, by Bruker (1 mentions)
Silica gel 60 f254, by Merck Group (1 mentions)
Avance 300, by Bruker (1 mentions)
Silica gel, by Merck Group (1 mentions)
Ftir 8100 spectrometer, by Shimadzu (1 mentions)
Jms gcmate mass spectrometer, by JEOL (1 mentions)
Rp 18 wf254s, by Merck Group (1 mentions)
Rid 10a refractive index detector, by Shimadzu (1 mentions)
Jnm eca600 spectrometer, by JEOL (1 mentions)
Silica gel 60n, by Kanto Chemical (1 mentions)
Ecx 400, by JEOL (1 mentions)
Ecs 400, by JEOL (1 mentions)
Jms 700tz mass spectrometer, by JEOL (1 mentions)
Chiralcel od h, by Daicel (1 mentions)
Chiralpak ad h, by Daicel (1 mentions)
3 protocols using sepa 300 digital polarimeter
1
Spectroscopic Analysis of Compound Characterization
2
NMR Characterization of Organic Compounds
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The 1H NMR (600 MHz, CDCl3), 13C NMR (150 MHz, CDCl3), and the 2D NMR spectra were recorded on a JEOL JNM-ECA 600 spectrometer (JEOL Ltd., Tokyo, Japan). All chemical shifts (δ) are given in ppm units with reference to TMS as an internal standard, and coupling constants (J) are reported in Hz. The IR spectra were taken on a Shimadzu FT-IR-8100 spectrometer. Specific rotations were measured on a Horiba SEPA-300 digital polarimeter (l = 5 cm). FAB-MS and HR-FAB-MS were recorded on a JEOL JMS-GC-MATE mass spectrometer. For chromatographic separations COSMOSIL-Pack type (C18-MS-II) (Inc., Cambridge, MA 02138, USA, 250 × 4.6 mm i.d.) and (250 × 20 mm i.d.) columns were used for analytical and preparative separations, respectively, with compound detection via a Shimadzu RID-10 A refractive index detector. For open silica gel column separations, normal-phase column chromatography employed BW-200 (Fuji Silysia, Aichi, Japan, 150–350 mesh) and reversed-phase column chromatography employed Chromatorex ODS DM1020 T (Fuji Silysia, Aichi, Japan, 100–200 mesh). TLC separations used precoated plates with silica gel 60 F254 (Merck, Pfizer, Sanofi, 0.25 mm) (ordinary phase) or reversed-phase precoated plates with silica gel RP-18 WF254S (Merck, Pfizer, Sanofi, 0.25 mm) with compounds observed by spraying with H2SO4-MeOH (1:9) followed by heating.
3
NMR Spectroscopy and HPLC Analysis Protocol
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1 H-NMR spectra were recorded on a JEOL ECX-400 (400 MHz) or JEOL ECS-400 (400 MHz) in CDCl 3 with tetramethylsilane (δ = 0.00) as internal standard. Chemical shifts are reported in part per million (ppm), and signal are expressed as singlet (s), doublet (d) , triplet (t), quartet (q), multiplet (m), and broad (br). 13 C-NMR spectra were recorded on a JEOL ECX-400 (100MHz) in CDCl 3 (δ = 77.00) with tetramethylsilane as an internal standard (δ = 0.0). Chemical shifts are reported in part per million (ppm). HPLC analysis was directly performed with chiral stationary phase column, Chiralpak AD-H or Chiralcel OD-H purchased from DAICEL Co., Ltd. High resolution mass spectra (HRMS) were recorded on a JEOL JMS 700TZ mass spectrometer at the Center for Instrumental Analysis, Hokkaido University. Optical rotations were measured on a HORIBA SEPA-300 digital polarimeter. Kanto Chemical silica gel 60N (particle size 0.063-0.210 mm) was used for flash column chromatography. RuCl and RuCl 2 (nbd)(MeCN) 2 17 were prepared by the literature procedure. BIPAM ligand (Me-BIPAM) were prepared according to our previous procedure. 18 Me-BIPAM was commercially available from Wako Pure Chemical Industries, Ltd. Phthalide was purchased from commercial source and substituted phthalides were synthesized according to known literature. 19
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