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4 protocols using am 600

1

Chromatographic Purification and NMR Analysis

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Column chromatographic procedures were performed using silica gel (80–120 mesh and 200–300 mesh, Qingdao Marine Chemical Co. Ltd., Qingdao, China) and Sephadex™ LH-20 gel (40–70 μm; Merck, Darmstadt, Germany), whereas precoated silica gel (GF254, Qingdao Marine Chemical Co. Ltd., Qingdao) plates were used for TLC analyses. Spots were visualized by heating silica gel plates sprayed with 10% H2SO4 in EtOH. UV spectra were recorded using a Waters UV-2401A spectrophotometer equipped with a DAD and a cell of 1 cm pathlength. Methanolic samples were scanned from 190 to 400 nm in 1 nm steps. Semipreparative HPLC was performed on an Agilent 1120 apparatus equipped with a UV detector and a reversed-phase C18 column (5 μm, 10 × 250 mm, Welch Ultimate XB-C18). 1D (1H, 13C) spectra of all compounds were recorded on Bruker AM-600, AM-500, and AM-400 NMR spectrometers (Bruker, Karlsruhe, Germany), with TMS as the internal reference. |Enzymatic activity experiments were performed using SpectraMax i3x (Molecular Devices, Austria).
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NMR Analysis of HPP-1 in D2O

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Twenty milligrams of HPP-1 were dissolved in 1.0 mL of D2O and placed in a nuclear magnetic tube. 1H-NMR and 13C-NMR analyses were conducted using a Bruker AM-600 nuclear magnetic resonance instrument.
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Synthesis and Characterization of Chiral Alcohols

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d-Valinol, d-phenylglycenol, d-leucinol, Ni (NO3)2·6H2O, Co(OAc)2.4H2O, Cu (OAc) 2.H2O, CuCl2·2H2O, CoCl2·6H2O, ZnCl2, and Cu(ClO4)2·6H2O were purchased from Acros. 1HNMR spectra were obtained using a Bruker AM-300 spectrometer. 1H and 13C NMR spectra were recorded using Bruker AM-500 and Bruker AM-600 spectrometers. Chemical shifts were reported in ppm (δ) with the solvent relative to tetramethylsilane (TMS) used as the internal standard (residual CHCl3, δH 7.26 ppm; CDCl3, C, 77 ppm). The following abbreviations were used to designate multiplicities: s = singlet, d = doublet, t = triplet, m = multiplet. Infrared spectra were recorded on a Mattson Galaxy Series FTIR 3000 spectrometer; peaks are reported in cm−1. Elemental analyses were performed on an Elemental Analyser AE-3000. The crystal structure was determined by a Gemini S Ultra diffractometer.
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4

Analytical characterization of compounds

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Optical rotations were measured at 25 °C on a Polaar 32 polarimeter. UV spectra were recorded on a Lightwave II + WPA 7126 V. 1.6.1 spectrophotometer. ECD spectra were measured at 25 °C on a JASCO J-810 spectropolarimeter. IR spectra were recorded with a PerkinElmer type 257 spectrometer. The NMR spectra were recorded on a Bruker AM-600 (600 MHz) NMR spectrometer equipped with a TCI 5 mm cryoprobe using CDCl as a solvent. The solvent signal was used as a reference. Sunfire preparative C columns (150 × 19 mm, i.d. 5 µm and 150 × 30 mm, i.d. 5 µm; Waters) were used for preparative HPLC separations using a Waters Delta Prep equipped with a binary pump (Waters 2525) and a UV-visible diode array detector (190-600 nm, Waters 2996). Silica 330 g, 120 g, and 24 g Grace cartridges were used for flash chromatography using an Armen Instrument spot liquid chromatography flash apparatus. Chemicals and solvents were purchased from Sigma-Aldrich. Create PDF in your applications with the Pdfcrowd HTML to PDF API PDFCROWD
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