All the reagents were purchased from Sigma Aldrich. The compounds were characterized by their physical constants data and spectro-analytical techniques. Melting points of the synthesized compounds were recorded in open capillaries using Gallenkamp melting point apparatus (MP-D). The chemical structure of synthesized compounds was characterized by infrared (IR), 1H nuclear magnetic resonance (1H NMR) and 13C nuclear magnetic resonance (13C NMR) spectroscopic techniques. The IR spectra were recorded on Thermoscientific Nicolet model 6700. 1H NMR and 13C NMR spectra were recorded on Bruker AV-300 MHz spectrometer using the desired solvent as indirect reference. UV-Vis spectroscopy was carried out at different temperatures using Shimadzu spectrophotometer, model Pharmaspec UV-1700. Surface morphology was studied by scanning electron microscopy (SEM) (JEOI, JSM-5910), operating at 20 kV with different magnification power.
Av 300 mhz spectrometer
Manufactured by Bruker
Sourced in Germany, United States, Switzerland
The AV-300 MHz spectrometer is a nuclear magnetic resonance (NMR) instrument manufactured by Bruker. It operates at a magnetic field strength of 300 MHz. The core function of the AV-300 MHz spectrometer is to perform high-resolution NMR spectroscopy for the analysis of chemical compounds.
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Lab products found in correlation
Nicolet model 6700, by Thermo Fisher Scientific (1 mentions)
Avance 3 hd 500 mhz nmr spectrometer, by Bruker (1 mentions)
Gpc system, by Malvern Panalytical (1 mentions)
Gpc max ve 2001, by Malvern Panalytical (1 mentions)
Tga dsc 3 module, by Mettler Toledo (1 mentions)
D glucose, by Merck Group (1 mentions)
Nadph, by Merck Group (1 mentions)
Avance 3, by Bruker (1 mentions)
Microtof q 2 mass spectrometer, by Bruker (1 mentions)
Silica gel, by Merck Group (1 mentions)
Autopol 1 automatic polarimeter, by Rudolph Research Analytical (1 mentions)
6 protocols using av 300 mhz spectrometer
1
Detailed Synthesis and Characterization
2
Polymer Analysis via GPC and NMR
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The homopolymers in the irradiated monomer solutions were analyzed by GPC and NMR. After irradiation, the acetone in the irradiated monomer solution was evaporated using a rotary evaporator at 40 °C for 10 min. About 5 μL of the acetone-free solution was directly injected into the GPC system to record the GPC curve. The GPC system (Hitachi High-Tech Sci. Corp., Tokyo, Japan) was equipped with a UV-detector (254 nm), a refractive index detector and two columns (Shodex, GPC KF-805L, Tokyo, Japan). The columns were controlled at 40 °C, and the THF eluent was fixed at a flow rate of 1.0 mL/min. The acetone-free solution was also diluted with CDCl3 containing small amount of tetramethylsilane. The tetramethylsilane was used as the internal standard for calibrating the chemical shift of the NMR spectra. About 0.5 mL of the resultant solution was transferred in an NMR tube to record the 1H NMR spectra using a Bruker AV 300 MHz spectrometer at room temperature.
3
NMR Characterization of Polymers
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The hollow fibers, sPESU10, and PSSNa were characterized by 1H NMR spectroscopy using a Bruker AV-300 MHz spectrometer and a Bruker Avance III HD 500 MHz NMR spectrometer (Ettlingen, Germany), respectively. In every experiment, tetramethylsilane (TMS) was used as an internal standard, and deuterated dimethyl sulfoxide (d6-DMSO) was used as a solvent to dissolve the samples in 5 mm O.D. sample tubes.
4
Spectroscopic and Thermal Analysis of Polymers
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The 1H NMR and 13C NMR spectra were recorded on a Bruker AV300 MHz spectrometer (Billerica, MA, USA) using CDCl3 as the solvent. The multiplicity of peaks is indicated as (bs) for broad signals, (s) singlet, (d) doublet, (t) triplet and (m) multiplet. The monomer conversion χ was evaluated by withdrawing aliquots of the reaction mixtures during the reaction to be analyzed by 1H NMR spectroscopy according to the literature [21 (link),24 (link)].
The molar masses were investigated by gel permeation chromatography (GPC) using a Viscotek GPC system using tetrahydrofuran (THF) as eluent. The GPC module comprised a pump and degasser system (GPCmax VE2001, Malvern, Worcs, UK; 1.0 mL min−1 flow rate), a Viscotek 302 TDA unit as detector (Malvern, Worcs, UK) and two columns for the analysis of different molar masses (2× PLGel Mix-B; dimensions 7.5 mm × 300 mm (all supplied by Malvern, Worcs, UK). The thermal characterization was performed with a TGA/DSC 3+ module (Mettler Toledo, Schwerzenbach, Switzerland). The thermal transitions were investigated from 25 °C to 360 °C under nitrogen flush (50 mL min−1), increasing the temperature with a rate of 10 °C min−1. The onset of decomposition was evaluated in a temperature range of 25 °C to 900 °C under air flush (50 mL min−1) with a temperature increasing rate of 10 °C min−1.
The molar masses were investigated by gel permeation chromatography (GPC) using a Viscotek GPC system using tetrahydrofuran (THF) as eluent. The GPC module comprised a pump and degasser system (GPCmax VE2001, Malvern, Worcs, UK; 1.0 mL min−1 flow rate), a Viscotek 302 TDA unit as detector (Malvern, Worcs, UK) and two columns for the analysis of different molar masses (2× PLGel Mix-B; dimensions 7.5 mm × 300 mm (all supplied by Malvern, Worcs, UK). The thermal characterization was performed with a TGA/DSC 3+ module (Mettler Toledo, Schwerzenbach, Switzerland). The thermal transitions were investigated from 25 °C to 360 °C under nitrogen flush (50 mL min−1), increasing the temperature with a rate of 10 °C min−1. The onset of decomposition was evaluated in a temperature range of 25 °C to 900 °C under air flush (50 mL min−1) with a temperature increasing rate of 10 °C min−1.
5
Synthetic and Biocatalytic Ketone/Alcohol Transformations
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Chemical reagents for the synthesis of ketones 3a-g and alcohols 4ag were purchased from Sigma-Aldrich. For the bioreduction experiments, D-glucose, NADH and NADPH were also acquired from Sigma-Aldrich, while glucose dehydrogenase (GDH-105) was obtained from Codexis Inc. and evo-1.1.200 from Evoxx Technologies GmbH. Made in house ADHs were overexpressed in E. coli: Ralstonia species (Ras-ADH), Sphingobium yanoikuyae (Sy-ADH), Thermoanaerobacter species (ADH-T), Lactobacillus brevis (Lb-ADH), Thermoanaerobacter ethanolicus (TeS-ADH) and Rhodococcus ruber (ADH-A).
Nuclear magnetic resonance (NMR) spectra ( 1 H and 13 C) were recorded on a Bruker AV300 MHz spectrometer. 125 Te NMR spectra were recorded on a Bruker Avance III at 9.4 T (400.13 MHz for 1 H NMR and 126.24 for 125 Te NMR) and the chemical shifts for 125 Te NMR were registered relative to an external standard diphenyl ditelluride (Ph2Te) at = 422 ppm. All chemical shifts (δ) are given in parts per million (ppm). Gas chromatography (GC) analyses were performed on an Agilent HP6890 GC chromatograph equipped with FID detector. Conversion rates measurements were performed on non-chiral GC column DB-1701 (30 m General procedures for the chemical synthesis of ketones 3a-g and alcohols 4a-g
Nuclear magnetic resonance (NMR) spectra ( 1 H and 13 C) were recorded on a Bruker AV300 MHz spectrometer. 125 Te NMR spectra were recorded on a Bruker Avance III at 9.4 T (400.13 MHz for 1 H NMR and 126.24 for 125 Te NMR) and the chemical shifts for 125 Te NMR were registered relative to an external standard diphenyl ditelluride (Ph2Te) at = 422 ppm. All chemical shifts (δ) are given in parts per million (ppm). Gas chromatography (GC) analyses were performed on an Agilent HP6890 GC chromatograph equipped with FID detector. Conversion rates measurements were performed on non-chiral GC column DB-1701 (30 m General procedures for the chemical synthesis of ketones 3a-g and alcohols 4a-g
6
Spectroscopic analysis of organic compounds
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The NMR spectra were recorded using Bruker AV 300 MHz spectrometer (Bruker, Fällanden, Switzerland) . Optical rotation was measured using a Rudolph Autopol I automatic polarimeter (Rudolph Research Analytical, Hackettstown, NJ, USA). Preparative middle pressure liquid chromatography (MPLC) was performed on an automatic flash chromatography device Ltd., Tianjin, China) . High-resolution electrospray ionisation mass spectra (HR-ESI-MS) were obtained using a Bruker micro TOF QII mass spectrometer (Bruker Daltonics, Fremont, CA, USA). Column chromatography was performed using silica-gel Branch of Qingdao Haiyang Chemical Co., Ltd., Qingdao, China) . was purchased from Merck KGaA (Darmstadt, Germany). TLC was performed with precoated silica-gel GF 254 glass plates (200 × 200 mm, Branch of Qingdao Haiyang Chemical Co., Ltd.) .
All other chemicals and solvents were analytical grade and used without further purification.
All other chemicals and solvents were analytical grade and used without further purification.
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