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The selective 1D INEPT (SINEPT) experiment allows to detect long-range proton-carbon connectivities from a 1D 13C spectrum. The experiment is very useful to assign quaternary carbon chemical shifts.REQUIREMENTS
Easy implementation on AVANCE spectrometers.VERSIONS
The 1D SINEPT pulse sequence ( 84JMR314-57 ) can easily derived from the conventional 1D refocused INEPT experiment by applying all proton pulses selective for an specific 1H resonance and optimizing the interpulse delays as a function of nJ(CH) (typically 5-10 Hz) (see refocused INEPT block).EXPERIMENTAL DETAILS
Several modified sequences has been proposed:
- The 1D SINEPT experiment has been used to detect non-protonated 15N nuclei ( 84JACS1150 ).
- A Selective 1D DEPT (SDEPT) experiment ( 92BMR263 and 94MRC343 ) has also been proposed with the same purpose. The pulse sequence is derived from the conventional DEPT experiment in which all proton pulses are made selective for a selected proton.
- A 2D selective J-INEPT experiment can be derived if the proton evolution period is made variable. This experiment allows to measure long-range 1H-13C coupling constants directly from a selective 2D J-resolved experiment.
- The experiment has been largely used for resonance assignment and structure elucidation. A review of applications on natural products has been published ( 91TET3521 ).
The 1D SINEPT experiment can be recorded in a fully automated way. Minor changes from a predefined parameter set are required. Important parameters to consider are:SPECTRAFor further details on practical implementation of the 1D SINEPT experiment on AVANCE spectrometers see Tutorial: Selective 1D INEPT experiment
- Selectivity of the selective pulses: the user must define the offset, the shape, the duration and the power level needed for a defined excitation profile.
- Optimization of the J-coupling interpulse delays as a function of nJ(CH) in the same way as described for the INEPT experiment. Standard values are 100 and 66 ms (5 Hz) for the refocusing and refocusing periods, respectively.
The 1D SINEPT experiment affords a 1D 1H-decoupled 13C spectrum only showing the 13C resonances whose are two or three bonds away of the selected 1H resonance. The intensities of these signals will depend of the delays optimization.RELATED TOPICS
2D COLOC and 2D HMBC experiment are useful alternative to trace out all long-range proton-carbon connectivities from a single 2D spectrum.