All chemicals, if not specified otherwise, were used as received without further purification. Poly (2,6-dimethyl-1,4-phenyleneoxide) (PPO) (Mn = 20,000, Đ = 2.5) was purchased from Polysciences Inc. and dried under vacuum at 60 °C overnight before use. Methanol (99.9%), ethanol (99.9%) and chloroform (99.8%) were purchased from Fisher Scientific. N-Bromosuccinimide (NBS) (99%), 2,2′-azobis(2-methylpropionitrile) (AIBN) (98%), tetrahydrofuran (THF, ACS, >99%), diethyl ether (>99%), chloroform-d (CDCl3-d, 99.9% D), Irgacure® 2959, D2O (99.9% D) and 1,2-dichloroethane (99.8%) were purchased from Sigma-Aldrich (Merck KGaA, Darmstadt, Germany). Dimethyl sulfoxide-d6 (DMSO-d6, 99.9%), N-methyl-2-pyrrolidone (NMP, reagent grade) were supplied from Acros Organics. Chlorobenzene (ACS reagent, ≥99.5%), diallymethylamine (97%) and piperidine (≥99%) were bought from ABCR GmbH. Allyl bromide (98%) and allyl chloride (98%) were bought from Alfa Aesar. The electrolytes MV and TMA-TEMPO were provided by JenaBatteries GmbH (Jena, Germany). FAA-3-50® was purchased from Fumatech BWT GmbH (Bietigheim-Bissingen, Germany).
Dimethyl sulfoxide d6
Manufactured by Thermo Fisher Scientific
Sourced in Belgium, United States
Dimethyl sulfoxide-d6 is a deuterated form of dimethyl sulfoxide, a commonly used solvent in chemical and biological research. It serves as a highly polar, aprotic solvent that is miscible with a wide range of organic solvents and water. Dimethyl sulfoxide-d6 is characterized by its high dielectric constant and low viscosity, making it a suitable choice for various applications in analytical and synthetic chemistry.
Automatically generated - may contain errors
Lab products found in correlation
Chloroform d, by Merck Group (2 mentions)
Methanol d4, by Merck Group (2 mentions)
Allyl chloride, by Thermo Fisher Scientific (1 mentions)
Ethanol, by Thermo Fisher Scientific (1 mentions)
Methanol, by Thermo Fisher Scientific (1 mentions)
1 2 dichloroethane, by Merck Group (1 mentions)
Irgacure 2959, by Merck Group (1 mentions)
Chloroform, by Thermo Fisher Scientific (1 mentions)
N bromosuccinimide, by Merck Group (1 mentions)
2 2 azobis 2 methylpropionitrile, by Merck Group (1 mentions)
Allyl bromide, by Thermo Fisher Scientific (1 mentions)
N methyl 2 pyrrolidone, by Thermo Fisher Scientific (1 mentions)
Tetrahydrofuran, by Merck Group (1 mentions)
Diethyl ether, by Merck Group (1 mentions)
Diallymethylamine, by ABCR (1 mentions)
Piperidine, by ABCR (1 mentions)
Deuterated water, by Merck Group (1 mentions)
Vnmrs spectrometer, by Agilent Technologies (1 mentions)
Sulfuric acid, by Thermo Fisher Scientific (1 mentions)
Ethylene glycol, by Thermo Fisher Scientific (1 mentions)
5 protocols using dimethyl sulfoxide d6
1
Synthesis and Characterization of Polymer Electrolytes
2
NMR Characterization of BPL Molecules
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Successful synthesis of BPL molecules was characterized by1HNMR. For1HNMR measurements, the products were dissolved in deuterated water (Cat. no. 151882; Sigma Aldrich), dimethyl sulfoxide‐d6 (Cat. no. 364650500; Acros Organic) or methanol‐d4 (Cat. no. 343803; Sigma Aldrich) at a concentration of ~1 wt. %. The spectra were recorded with a 500 MHz Agilent/ Varian VNMRS spectrometer at room temperature.
3
NMR Spectroscopic Analysis of Purified Products
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Nuclear magnetic resonance (NMR) spectra
were obtained using a Bruker AVANCE Digital 400 MHz NMR spectrometer
coupled to a BACS 1 automatic sample changer. The spectrometer is
equipped with a 5 mm PABBO BB-1H/D Z-GRD probe. The 1H
spectra of the purified products (6–8 mg) were recorded in
(500–600 μL) methanol-d4 (Alfa
Aesar, 99.8% D) or dimethyl sulfoxide-d6 (Acros Organics, 99.5% D) with average 16 scans, and for 13C spectra, average 1000 scans were performed for each sample. Chemical
shifts were reported in parts per million (ppm), with the residual
undeuterated solvent peaks as an internal reference for 1H NMR: CD3OD (3.31 and 4.78 ppm) and DMSO (2.50 ppm).
Multiplicities were reported as singlet (s), doublet (d), triplet
(t), or multiplet (m), and coupling constants (J) are given in Hertz
(Hz).
were obtained using a Bruker AVANCE Digital 400 MHz NMR spectrometer
coupled to a BACS 1 automatic sample changer. The spectrometer is
equipped with a 5 mm PABBO BB-1H/D Z-GRD probe. The 1H
spectra of the purified products (6–8 mg) were recorded in
(500–600 μL) methanol-d4 (Alfa
Aesar, 99.8% D) or dimethyl sulfoxide-d6 (Acros Organics, 99.5% D) with average 16 scans, and for 13C spectra, average 1000 scans were performed for each sample. Chemical
shifts were reported in parts per million (ppm), with the residual
undeuterated solvent peaks as an internal reference for 1H NMR: CD3OD (3.31 and 4.78 ppm) and DMSO (2.50 ppm).
Multiplicities were reported as singlet (s), doublet (d), triplet
(t), or multiplet (m), and coupling constants (J) are given in Hertz
(Hz).
4
Characterization of Imidazolium Polymers
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1H-NMR and 19F-NMR spectra were obtained using a Bruker DRX-300 spectrometer and a Brucker Advance III 500 spectrometer, respectively. Monomeric samples were dissolved in chloroform-d (Aldrich, St. Louis, MO, USA 99.8 atom % D, 0.05% v/v TMS) or methanol-d4 (Aldrich, St. Louis, MO, USA, 99.96 atom % D). Polymers were dissolved in dimethylsulfoxide-d6 (ACROS Organics, Geel, Belgium, 99.9 atom % D). The 19F NMR spectrum of poly(1-butyl-2,3-dimethyl-4-vinylimidazolium triflate) shows a single sharp peak at ~78 ppm. When fully ion-exchanged to poly(1-butyl-2,3-dimethyl-4-vinylimidazolium hexafluorophosphate), no trace of a peak at ~78 ppm is observed, as it is replaced by a doublet centered at ~75 ppm with a coupling constant of about 711 Hz. This splitting arises by virtue of coupling between 19F and 31P. These spectra are included in the Supplementary Information .
5
Synthesis of 2,5-Furandicarboxylic Acid
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2,5-Furandicarboxylic acid (99.27% by HPLC) was purchased from Chem-Impex International Inc. (Illinois, USA). Terephthalic acid (99+%) and dimethyl sulfoxide-d6 (99.5 + atom% D) were purchased from Acros Organics (New Jersey, USA). Ethylene glycol (certified ACS), dimethyl sulfoxide (certified ACS), sodium hydroxide pellets (CAS grade), and sulfuric acid (certified, 72% w/w, 24.0 N, ±0.1 N (12 M)) were purchased from Fisher Scientific (New Hampshire, USA). All the reagents were used as received without further purification.
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