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.
Unity inova 300
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.
4 protocols using unity inova 300
Thermal Stability of Terpene Isomers
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.
NMR and HRMS Characterization of Compounds
NMR Spectroscopy of Organic Compounds
Characterization of Air-Sensitive Compounds
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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