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4 protocols using ftir 8100 spectrometer

1

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.
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2

Analytical Techniques for Compound Characterization

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For specific rotation, a Horiba SEPA-300 digital polarimeter (5 cm) was used and IR data was collected from a Shimadzu FTIR-8100 spectrometer. For mass spectrometry measurements, IMS was performed on a Finnegan LCQ ion trap mass spectrometer and HR-EI-MS experiments were performed on Fourier transform ion cyclotron mass spectrometer. EI-MS experiments were performed a JEOL JMS-GCMATE mass spectrometer. Using tetramethylsilane as an internal standard, the 1H (600 MHz) and 13C (150 MHz) NMR spectra were achieved on a JEOL JNM-ECA 600 spectrometer. Compound separation for analytical and preparative separation was carried out using YMC-Pack ODS-A (250 × 4.6 mm i.d.) and (250 × 20 mm i.d.) columns, respectively. Purification was performed using a Shimadzu HPLC system furnished with a RID-10A refractive index detector. Fuji Silysia Chemical, Ltd.'s normal-phase silica BW-200 (Fuji Silysia Chemical, Ltd., 150–350 mesh) and Chromatorex's ODS reverse phase DM1020T (Fuji Silysia Chemical, Ltd., 100–200 mesh) were used for chromatography separations (Fuji Silysia Chemical, Ltd., 100–200 mesh). Additionally, silica gel 60 F254 (Merck, 0.25 mm) and RP-18 WF254 were used (Merck, 0.25 mm) for TLC analysis with compound visualization by with H2SO4–MeOH (1 : 9) spray followed by heating.
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3

Characterization of Organic Compounds

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Specific rotation was measured with a Horiba SEPA-300 digital polarimeter (Kyoto, Japan, l = 5 cm) and IR spectra were collected on a Shimadzu FTIR-8100 spectrometer (Kyoto, Japan). For X-ray, a Bruker SMART-APEX II ULTRA (Billerica, MA, USA) was used. ESI-MS and HR-ESI-MS were carried out using a Thermo Fisher Scientific LTQ Orbitrap XL mass spectrometer (Waltham, MA, USA), and 1H (600 MHz) and 13C (150 MHz) NMR spectra were recorded on a JEOL JNM-ECA 600 spectrometer (Tokyo, Japan) with tetramethylsilane as an internal standard. Purification was run on a Shimadzu HPLC system equipped with a RID-10A refractive index detector and compound separation was performed on YMC-Pack ODS-A (Tokyo, Japan, 250 × 4.6 mm i.d.) and (250 × 20 mm i.d.) columns for analytical and preparative separation, respectively. Chromatography separation included normal-phase silica BW-200 (Fuji Silysia Chemical, Ltd., Kasugai, Japan, 150–350 mesh) and ODS reverse phase Chromatorex DM1020T (Fuji Silysia Chemical, Ltd., 100–200 mesh) columns as well as silica gel 60F254 (Merck, Darmstadt, Germany, 0.25 mm) and RP-18 WF254S (Merck, 0.25 mm) TLC plates with spots developed with heating of H2SO4-MeOH (1:9) sprayed plates.
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4

Analytical Techniques for Compound Characterization

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The following instruments were used to obtain physical data: UV spectra, UV-1600 spectrometer (Shimadzu Co., Kyoto, Japan); IR spectra, FTIR-8100 spectrometer (Shimadzu Co.); EI-MS and HR-EI-MS, JMS-GCMATE mass spectrometer (JEOL Ltd., Tokyo, Japan); 1 H-NMR spectra, JNM-ECA500 (500 MHz), and JNM-ECS400 (400 MHz) spectrometers (JEOL); 13 (link) C-NMR spectra, JNM-ECA500 (125 MHz), and JNM-ECS400 (100 MHz) spectrometers (JEOL Ltd.) with tetramethylsilane as an internal standard; HPLC detector, SPD-10Avp UV-VIS detector (Shimadzu Co.); HPLC column, Cosmosil 5C 18 -MS-II (Nacalai Tesque, Inc., Kyoto, Japan), 4.6×250 mm i.d. and 20×250 mm i.d. for analytical and preparative studies, respectively.
The following experimental conditions were used for chromatography (CC): ordinary-phase silica gel column chromatography, silica gel 60N (Kanto Chemical Co., Tokyo,
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