The DPX-400 is a nuclear magnetic resonance (NMR) spectrometer instrument manufactured by Bruker. It is designed to perform high-resolution NMR analysis of chemical samples. The core function of the DPX-400 is to generate and detect radio frequency (RF) signals to measure the magnetic properties of atomic nuclei within a sample, providing detailed structural information about the sample's chemical composition.
All chemicals were purchased from commercial sources or provided by Pfizer and used without further purification. Substrates 2b–d were synthesized according to the reported procedure. Unless stated otherwise, all column purification were performed on a Biotage Selekt Flash Chromatography, eluted with ethyl acetate: hexane, 0–15% gradient, detected by UV absorption at 254 nm. Thin layer chromatography (TLC) was carried out using Merck Millipore TLC silica gel 60 F254 glass plates. 1H, 13C, and 19F NMR spectra were measured on a Bruker DPX-400 instrument (operating at 400 MHz for 1H, 100 MHz for 13C, and 375 MHz for 19F) or a Bruker DPX-500 instrument (operating at 500 MHz for 1H and 125 MHz for 13C).
Ren X., Couture B.M., Liu N., Lall M.S., Kohrt J.T, & Fasan R. (2022). Enantioselective Single and Dual α-C–H Bond Functionalization of Cyclic Amines via Enzymatic Carbene Transfer. Journal of the American Chemical Society, 145(1), 537-550.
All reactions were carried out under a nitrogen atmosphere using standard Schlenk techniques unless otherwise stated. Reagent-grade solvents were dried using appropriate drying agents and distilled by standard methods prior to use. Ru3(CO)12 was purchased from Strem Chemicals Inc. and used without further purification. 2-Vinylpyrazine and dppm were purchased from Acros Organics and used as received. Ru3(CO)10(μ-dppm) was prepared according to a literature method.27 Products were separated without any special precautions on TLC plates coated with 0.25 mm silica gel (HF254-type 60, E. Merck, Germany). IR spectra were recorded on a Shimadzu FTIR Prestige 21 spectrophotometer and NMR spectra on a Bruker DPX 400 instrument. All chemical shifts are reported in δ units and are referenced to the residual protons of the deuterated solvents (1H) or to external H3PO4 (31P), whose chemical shift is assigned to δ = 0.0. Elemental analyses were performed by the Microanalytical laboratory of Wazed Miah Science Research Centre at Jahangirnagar University.
Hossain M.M., Akter N., Ghosh S., Nesterov V.N., Richmond M.G., Hogarth G, & Kabir S.E. (2019). New molecular architectures containing low-valent cluster centres with di- and trimetalated 2-vinylpyrazine ligands: synthesis and molecular structures of Ru5(CO)15(μ5-C4H2N2CH CH)(μ-H)2 and Ru8(CO)24(μ7-C4H2N2CHC)(μ-H)3. RSC Advances, 9(36), 21025-21030.
Unless otherwise noted, all reactions were carried out under a nitrogen atmosphere using standard Schlenk techniques. Reagent-grade solvents were dried using appropriate drying agents and distilled prior to use by standard methods. Infrared spectra were recorded on a Shimadzu FTIR 8101 spectrophotometer. NMR spectra were recorded on a Bruker DPX 400 instrument. Mass spectra were recorded on a Varian Mat 312 mass spectrometer. Elemental analyses were performed by Microanalytical Laboratories, University College London. Collman’s reagent and phosphines were purchased from Strem Chemical Inc. and used without further purification.
Rahaman A., Ghosh S., Unwin D.G., Basak-Modi S., Holt K.B., Kabir S.E., Nordlander E., Richmond M.G, & Hogarth G. (2014). Bioinspired Hydrogenase Models: The Mixed-Valence Triiron Complex [Fe3(CO)7(μ-edt)2] and Phosphine Derivatives [Fe3(CO)7–x(PPh3)x(μ-edt)2] (x = 1, 2) and [Fe3(CO)5(κ2-diphosphine)(μ-edt)2] as Proton Reduction Catalysts. Organometallics, 33(6), 1356-1366.
All chemicals were purchased from commercial sources or provided by Pfizer and used without further purification. Substrates 2b-2d were synthesized according to the reported procedure. Unless stated otherwise, all column purification were performed on a Biotage Selekt Flash Chromatography, eluted with ethyl acetate: hexane, 0-15% gradient, detected by UV absorption at 254nm. Thin Layer Chromatography (TLC) was carried out using Merck Millipore TLC silica gel 60 F254 glass plates. 1H, 13C, and 19F NMR spectra were measured on a Bruker DPX-400 instrument (operating at 400 MHz for 1H, 100 MHz for 13C, and 375 MHz for 19F) or a Bruker DPX-500 instrument (operating at 500 MHz for 1H and 125 MHz for 13C).
Ren X., Couture B.M., Liu N., Lall M.S., Kohrt J.T, & Fasan R. (2022). Enantioselective Single and Dual α-C–H Bond Functionalization of Cyclic Amines via Enzymatic Carbene Transfer. Journal of the American Chemical Society, 145(1), 537-550.
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