Tetrahydrofuran, 1,2-dimethoxyethane and diglyme were dried and distilled from sodium/benzophenone under Ar. Reagents were used as supplied without purification unless stated otherwise. All operations were performed under argon using Schlenk techniques unless stated otherwise. Sodium hydride (60% oil dispersion) was washed with hexane three times under Ar before use. (Trifluoromethyl)trimethylsilane was purchased from Oakwood Chemical (Estill, SC, USA). (Difluoromethyl)trimethylsilane [23 (link)], (bromodifluoromethyl)trimethylsilane [24 (link)], (chlorodifluoromethyl)trimethylsilane [25 (link)], (tribromomethyl)trimethylsilane [26 ] and (trichloromethyl)trimethylsilane [27 (link)] were prepared according to reported procedures. 1H, 11B and 19F NMR spectra were recorded on Bruker Avance-III 300 MHz instrument in CDCl3 or CDC3N. Chemical shifts are reported in ppm.
Avance 3 300 mhz instrument
Manufactured by Bruker
Sourced in United States
The Avance-III 300 MHz instrument is a nuclear magnetic resonance (NMR) spectrometer produced by Bruker. It operates at a magnetic field strength of 300 MHz and is designed for high-resolution NMR analysis of chemical and biological samples.
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Lab products found in correlation
3 protocols using avance 3 300 mhz instrument
1
Synthesis and NMR Characterization of Halomethyl-Substituted Silanes
2
Synthesis and Characterization of Silane Cross-Linking Agent
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Example 4
19.79 g of KBE-9007 (3-isocyanatopropyltriethoxysilane), 12.80 g of PEG-400 and 0.57 g of DBTDL were placed in a 1000 ml flask, and diluted with 300 g of tetrahydrofuran. After stirring at room temperature until all of the reactants were confirmed to be consumed by TLC, the reaction solvent was completely removed under reduced pressure.
28 g of a liquid product having a purity of 95% or more was separated at a yield of 91% through column chromatography under a developing solution (dichloromethane: methyl alcohol=30:1) to obtain the above-mentioned silane cross-linking agent.
Herein, the solid state 29Si NMR analysis of the silane cross-linking agent was performed using a Bruker AVANCE III 300 MHz instrument and a 7 mm MAS probe in a static condition. By calculating integral values, it was confirmed that a ratio of functional groups represented by the following Chemical Formula 1 to functional groups represented by the following Chemical Formulae 1 to 4 of the siloxane functional groups was about 95 mol % (the description of the functional groups represented by the following Chemical formulae 1 to 4 is as described above).
3
Purification and Characterization of Product A
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Product A was purified through preparative LC utilizing an XBridge C18 column (50 mm x 250 mm, 5 µm particle size; Waters Corp., USA). Elution was carried out with a solvent composed of 5% H2O, 47.5% MeOH, and 47.5% EtOH at a flow rate of 70 ml/min. Fractions eluting between 7 and 8 min were collected and subsequently concentrated using a centrifugal evaporator (EYELA N1000V, Japan) to obtain a viscous and colorless liquid.
The purity of Product A was assessed by HPLC using the aforementioned analysis conditions. NMR spectra were acquired on an Avance III 300 MHz instrument (Bruker BioSciences Corp., USA) using deuterated chloroform (CDCl3) as solvent. Additionally, LC-MS analysis was performed utilizing a LC-MS 8050 system (Shimadzu) in positive electron spray ionization (ESI) mode, with a mass scan range of m/z 100-1500.
The purity of Product A was assessed by HPLC using the aforementioned analysis conditions. NMR spectra were acquired on an Avance III 300 MHz instrument (Bruker BioSciences Corp., USA) using deuterated chloroform (CDCl3) as solvent. Additionally, LC-MS analysis was performed utilizing a LC-MS 8050 system (Shimadzu) in positive electron spray ionization (ESI) mode, with a mass scan range of m/z 100-1500.
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