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4 protocols using ftir 300e infrared spectrophotometer

1

Comprehensive Characterization of Compound

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The 1H, 13C and 2D NMR spectra were recorded at 400 and 100 MHz, respectively, using TMS as internal standard in methanol-d4, using the residual solvent peak (δH= 3.34 and δC= 49.9) as references, on Bruker Avance III 400 MHz with BBFO Smart Probe and Bruker 400 MHz AEON Nitrogen-Free Magnet (Bruker AG, Switzerland). Carbon multiplicities were determined using DEPT-Q experiments. The optical rotation values were determined using a Jasco P-1020 polarimeter (Easton, MD, USA). The UV spectrum in methanol was obtained using a Shimadzu UV 2401PC spectrophotometer. The IR spectra were obtained using a Jasco, FT IR 300E infrared spectrophotometer. ESI-MS data were obtained using a Thermo Scientific LTQ/XL Orbitrap (Waltham, MA USA). Column chromatography was performed using silica gel 60 (63–200 µm, Fluka, Sigma-Alderich, Germany); Polyamide-6 (50–160 µm, Sigma-Aldrich, Germany) and Sephadex LH-20 (Sigma-Aldrich, Germany). HPLC separations were conducted using an Agilent 1260 Infinity preparative pump (G1361A), Agilent 1260 Diode array detector VL (G1315 D), Agilent 1260 Infinity Thermostand column compartment (G1361 A) and Agilent 1260 Infinity preparative Autosampler (G2260A). YMC-Pack ODS-A A-324 column (i.d. 10 × 300 mm, YMC, Kyoto, Japan).
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2

Comprehensive NMR and Spectral Analysis

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The 1H, DEPT-Q, and 2D NMR spectra were recorded at 400 and 100 MHz, respectively; using tetramethylsilane (TMS) as the internal standard in methanol-d4, using the residual solvent peak (δH = 3.34 & δC = 49.9) as references, on Bruker Avance III 400 MHz with a BBFO Smart Probe and Bruker 400 MHz EON Nitrogen-Free Magnet (Bruker AG, Billerica, MA, USA). Carbon multiplicities were determined using the DEPT-Q experiment. The optical rotation in methanol was obtained using a Perkin-Elmer 343 polarimeter (PerkinElmer Inc., Waltham, MA, USA). The UV spectrum in methanol was obtained using a Shimadzu UV 2401PC spectrophotometer (Shimadzu Corporation - UV-2401PC/UV-2501PC, Kyoto, Japan). The IR spectra were obtained using a Jasco FTIR 300E infrared spectrophotometer. HRESIMS data were obtained using an Acquity Ultra Performance Liquid Chromatography system coupled to a Synapt G2 HDMS quadrupole time-of-flight hybrid mass spectrometer (Waters, Milford, MA, USA).
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3

NMR and Spectroscopic Characterization

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Proton 1H and Distortionless Enhancement by Polarization Transfer-Q (DEPT-Q) 13C NMR spectra were recorded at 400 and 100 MHz, respectively. Tetramethylsilane (TMS) was used as an internal standard in methanol-d4 (CD3OD-d4) and dimethyl sulfoxide (DMSO-d6), using the residual solvent peaks (δH = 3.34, 4.78 and δC = 49.9; and δH = 2.50 and δC = 39.5) as references. Measurements were performed in a Bruker Advance III 400 MHz with a BBFO smart probe and a Bruker 400 MHz EON nitrogen-free magnet (Bruker AG, Billerica, MA, USA). Carbon multiplicities were determined using a DEPT-Q experiment. The ultraviolet radiation (UV) spectrum in methanol was obtained using a Shimadzu UV 2401PC spectrophotometer (Shimadzu Corporation – UV-2401PC/UV-2501PC, Kyoto, Japan). Infrared (IR) spectra were measured using a Jasco FTIR 300E infrared spectrophotometer. HRESIMS data were obtained using an Acquity ultra performance liquid chromatography system coupled to a Synapt G2 HDMS quadrupole time-of-flight hybrid mass spectrometer (Waters, Milford, MA, USA).
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4

Comprehensive NMR and Spectroscopic Characterization

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Proton 1H and Distortionless Enhancement by Polarization Transfer-Q (DEPT-Q) 13C NMR spectra were recorded at 400 and 100 MHz, respectively. Tetramethylsilane (TMS) was used as an internal standard in CDCL3-d and CD3OD-d4, utilizing residual solvent peaks (δH = 7.26; and δC 77.2) and (δH = 3.34; 4.78; and δC 49.9) as references, respectively. Measurements were performed on a Bruker Advance III 400 MHz with BBFO Smart Probe and a Bruker 400 MHz EON Nitrogen-Free Magnet (Bruker AG, Billerica, MA, USA). Carbon multiplicities were determined using a DEPT-Q experiment. The ultraviolet radiation (UV) spectrum in methanol was obtained using a Shimadzu UV 2401PC spectrophotometer (Shimadzu Corporation-UV-2401PC/UV-2501PC, Kyoto, Japan). Infrared (IR) spectra were measured using a Jasco FTIR 300E infrared spectrophotometer. HRESIMS data were obtained using an Acquity Ultra Performance Liquid Chromatography system coupled with a Synapt G2 HDMS quadrupole time-of-flight hybrid mass spectrometer (Waters, Milford, MA, USA).
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