All manipulations were carried out under an argon atmosphere using either Schlenk line techniques or glove boxes. Solvents were purified by the Ultimate Solvent System, Glass Contour Company (Nikko Hansen & Co., Osaka, Japan) [41 (link)]. 1H-, 13C-, 28Si-, and 31P-NMR spectra were measured on a JEOL AL-300 spectrometer (JEOL Ltd., Tokyo, Japan) or a Bruker Avance-600 spectrometer (Bruker, Billerica, MA, USA). High-resolution mass spectra (HRMS) were measured on a Bruker micrOTOF focus-Kci mass spectrometer (on ESI-positive mode) (Bruker). Elemental analysis was carried out by using Micro Corder JM10 (J-Science Lab Co., Ltd., Kyoto, Japan) at the Microanalytical Laboratory, Institute for Chemical Research, Kyoto University. TMS3SiSiCl3 was prepared according to literature procedure [33 (link)].
Al 300 spectrometer
Manufactured by JEOL
Sourced in Japan
The AL-300 spectrometer is a laboratory instrument designed for the analysis and characterization of materials. It is capable of performing nuclear magnetic resonance (NMR) spectroscopy, a widely used technique in various scientific fields. The AL-300 measures the magnetic properties of atomic nuclei within a sample, providing detailed information about the chemical structure and composition of the material under investigation.
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Lab products found in correlation
Avance 600 spectrometer, by Bruker (1 mentions)
Jms 700 spectrometer, by JEOL (1 mentions)
Lambda 400 spectrometer, by JEOL (1 mentions)
Kieselgel 60 f254 plate, by Merck Group (1 mentions)
8453 diode array spectrophotometer, by Hewlett-Packard (1 mentions)
Tlc silica gel 60 f254, by Merck Group (1 mentions)
4 protocols using al 300 spectrometer
1
Synthesis and Characterization of Organosilicon Compounds
2
Characterization of Organophosphorus Compounds
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All solution‐phase reactions were conducted under an argon atmosphere. 1H NMR spectra were obtained at 300 MHz on a JEOL Al300 spectrometer and at 400 MHz on a JEOL Lambda 400 spectrometer with tetramethylsilane (TMS) as an internal standard (δ 0.0) in CDCl3. 31P NMR spectra were obtained at 162.0 MHz on a JEOL Lambda 400 spectrometer with 85 % H3PO4 (δ 0.0) as an external standard. 19F NMR spectra were obtained at 376.3 MHz on a JEOL Lambda 400 spectrometer. Mass spectra were recorded on a JMS‐700 spectrometer (JEOL) with trifluoroacetic acid as an external standard (δ−76.5). Mass spectra were recorded on a 910‐MS FTMS system (Varian) or a Voyager System 4327 (Applied Biosystems). Analytical TLC was performed on Merck Kieselgel 60‐F254 plates. Silica gel column chromatography was carried out using silica gel 60 n (63–210 μm or 40–50 μm) as a neutral silica gel, and Chromatorex NH‐DM1020 as an NH silica gel. Gel filtration chromatography was conducted using Sephadex® LH‐20. RP‐HPLC was carried out using a μBondasphere 5 μm C18, 100 Å, 3.9 mm × 150 mm (Waters). Organic solvents were purified and dried according to the appropriate procedures. Anomeric ratio was calculated from relative peak areas in 19F NMR and 31P NMR.
3
Synthesis and Characterization of Ferrocenes
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Chemicals were purchased from commercial sources and used without further purification, unless otherwise noted. Perchloric acid (HClO4, 70%), trifluoroacetic acid (TFA), ferrocene (Fc), and 1,1-dimethylferrocene (Me2Fc) were purchased from Wako Pure Chemical Industries Ltd. Octamethylferrocene (Me8Fc) and decamethylferrocene (Me10Fc) were received from Sigma Aldrich. Fc, Me2Fc, Me8Fc, and Me10Fc were purified by sublimation or recrystallization from ethanol. Benzonitrile (PhCN) used for spectroscopic and electrochemical measurements was distilled over phosphorus pentoxide prior to use.48 [14]Triphyrin(2.1.1) [HTrip] was synthesized according to the reported procedure.41 (link) Fe(ii )(TMC)(OTf)2 (TMC = 1,4,8,11-tetramethyl-1,4,8,11-tetraazacyclotetradecane; OTf = CF3SO3) was prepared according to a literature method.43 (link) Tetra-n-butylammonium hexafluorophosphate (TBAPF6) was twice recrystallized from ethanol and dried in vacuo prior to use. 1H NMR spectra (300 MHz) were recorded on a JEOL AL-300 spectrometer at room temperature and chemical shifts (ppm) were determined relative to tetramethylsilane (TMS). UV-vis absorption spectroscopy was carried out on a Hewlett Packard 8453 diode array spectrophotometer at room temperature using a quartz cell (light path length = 1 cm).
4
Interaction of 2-APB and H2O2 Analysis
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To examine the direct interaction between 2-APB and H2O2, 1H-NMR measurement and thin-layer chromatography were performed [28 ] [29 ]. Five milligrams of 2-APB (0.0222 mmol) were dissolved in methanol-d4 (0.6 mL) in an NMR tube at room temperature, and the mixture was subjected to 1H-NMR analysis to obtain an authentic spectrum (spectrum A). H2O2 (31% w/v, 25 μL, 0.222 mmol) was then added to this mixture. After shaking for a few seconds, the mixture was subjected to the 1H-NMR analysis and the second spectrum was recorded in 5 min (spectrum B). After 60 min, the mixture was analyzed to obtain the third spectrum (spectrum C). All 1H-NMR spectra were recorded on a 300 MHz JEOL AL-300 spectrometer in the deuterated solvent, and the chemical shifts were reported with a residual peak of CD2HOD as an internal standard. The reaction products were further examined by thin-layer chromatography (TLC) using TLC plates (TLC silica gel 60 F254; Merck Millipore, Billerica, MA).
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