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Unity inova 300

Manufactured by Agilent Technologies
Sourced in China, United Kingdom

The Unity Inova 300 is a nuclear magnetic resonance (NMR) spectrometer designed for analytical and research applications. It provides a high-resolution analysis of chemical compounds, allowing users to identify and characterize their molecular structures. The Unity Inova 300 operates at a magnetic field strength of 7.05 Tesla, which enables it to perform precise measurements of nuclear magnetic properties.

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4 protocols using unity inova 300

1

Thermal Stability of Terpene Isomers

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The standards for linalool oxide (furanoid, cis and trans), pseudoionone (cis and trans) and farnesol (E,Z; Z,E; and E,E) contains a mixture of isomers. The standards were diluted to a concentration of 10,000 mg/L in deuterated chloroform. The ratio of cis:trans was identified using 1H nuclear magnetic resonance (NMR) spectroscopy. NMR spectra were recorded on a Varian unity Inova 300 (1H; 300.08 MHz) NMR spectrometer equipped with the sample injector at 30 °C.
Diastereomers containing the cis/trans double bond may be susceptible to interconversion under thermal treatment [20 (link)]. Terpenes in particular may be susceptible to this transformation, as demonstrated by multiple sources of literature [20 (link),57 (link),58 (link),59 (link)]. Hence, to confirm the thermal stability of the cis/trans diastereomers at elevated temperatures (as the samples are introduced into the GC inlet at 250 °C), the ratio was also determined by GC–FID. The samples diluted to a concentration of 20 mg/L with dichloromethane and analysed by GC–FID. The ratio obtained from 1H NMR was compared to the ratio of cis and trans diastereomers identified by GC–FID. Importantly, no cis:trans inter-conversion was observed. The cis:trans ratio of linalool oxide (furanoid) and pseudoionone were 57:43 and 29:71 respectively.
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2

NMR and HRMS Characterization of Compounds

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All chemicals (reagent grade) used were purchased from Sigma–Aldrich (USA) and Sinopharm Chemical Reagent Co. Ltd. (China).1H NMR spectra were measured on Varian Unity Inova 300 or 400 MHz NMR Spectrometers at 25 °C and referenced to TMS. Chemical shifts are reported in ppm using the residual solvent line as internal standard. Splitting patterns are designed as s, singlet; d, doublet; t, triplet; m, multiplet. HRMS spectra were acquired on an Agilent Technologies 6220 Accurate-Mass TOF LC/MS. Analytical thin-layer chromatography (TLC) was performed on the glass-backed silica gel sheets (silica gel 60 Å GF254). All compounds were detected using UV light (254 or 365 nm). Analytical HPLC was conducted on SHIMADZU LC-20AD. Prior to Ki measurement, all compounds were determined to be >95% pure by HPLC based on the peak area percentage.
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3

NMR Spectroscopy of Organic Compounds

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1H, 13C, 1H-1H correlation spectroscopy (COSY), and 1H-13C gradient heteronuclear single quantum coherence adiabatic version (gHSQCad) spectra were recorded in DMSO-d6 or in D2O on a Varian Unity Inova 300 instrument (Oxford, UK) in the pulse Fourier-transform mode with a relaxation delay of 5 s, and an acquisition time of 3 s. Tetramethylsilane (TMS, δ = 0) and 3-trimethylsilyl-2,2′,3,3′-d4-propanoic acid sodium salt (TMSPA, δ = 0) were used as internal chemical-shift standards in DMSO-d6 and D2O, respectively.
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4

Characterization of Air-Sensitive Compounds

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All reactions involving air-sensitive compounds were carried out under an atmosphere of dry nitrogen or argon using either Schlenk techniques or a glove box. Solvents were dried using a column solvent purification system [59] .
1H (300 MHz), 13C (75.4 MHz), and 29Si (59.3 MHz), NMR spectra were recorded on a Varian Unity INOVA 300. Samples for 29Si spectra were either dissolved in deuterated solvents or in cases of reaction samples measured with a D2O capillary in order to provide an external lock frequency signal. To compensate for the low isotopic abundance of 29Si the INEPT pulse sequence [60] , [61] was used for the amplification of the signal. If not noted otherwise the used solvent was C6D6 and all samples were measured at rt. Mass spectra were run on an HP 5971/A/5890-II GC/MS instrument (HP 1 capillary column, length 25 m, diameter 0.2 mm, 0.33 μm poly(dimethylsiloxane)). Elementary analysis was carried using a Heraeus VARIO ELEMENTAR EL apparatus. UV spectra were measured on a Perkin Elmer Lambda 35 spectrometer using spectroscopy grade pentane as solvent.
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