Extracting Scalar Couplings From Complex ¹ H NMR Spectra Using a Simple 2D J‐Resolved Sequence

Measurement of scalar couplings between protons is a very challenging task because of complex multiplet patterns and severe overlapping of these multiplets in congested 1D spectra. Numerous 2D J-resolved sequences now exist that utilize either the Zangger-Sterk or PSYCHE or z-filter elements along with selective refocusing and pure-shift schemes to generate high-resolution phase-sensitive spectra with simple doublets in <mml:math xmlns:mml="http://www.w3.org/1998/Math/MathML"> <mml:semantics> <mml:mrow> <mml:msub><mml:mrow><mml:mi>F</mml:mi></mml:mrow> <mml:mrow><mml:mn>1</mml:mn></mml:mrow> </mml:msub> </mml:mrow> <mml:annotation>$$ {F}_1 $$</mml:annotation></mml:semantics> </mml:math> dimension. Herein, we present a 2D J-resolved sequence that employs a simple element consisting of hard pulses and inter-pulse delays to generate phase-sensitive spectra. This simple element in combination with selective refocusing eliminates all the undesired components including the intense axial peaks, thus provides clean 2D J-resolved spectra with signals of only two targeted protons with simple doublets in <mml:math xmlns:mml="http://www.w3.org/1998/Math/MathML"> <mml:semantics> <mml:mrow> <mml:msub><mml:mrow><mml:mi>F</mml:mi></mml:mrow> <mml:mrow><mml:mn>1</mml:mn></mml:mrow> </mml:msub> </mml:mrow> <mml:annotation>$$ {F}_1 $$</mml:annotation></mml:semantics> </mml:math> dimension and full multiplets of target protons in <mml:math xmlns:mml="http://www.w3.org/1998/Math/MathML"> <mml:semantics> <mml:mrow> <mml:msub><mml:mrow><mml:mi>F</mml:mi></mml:mrow> <mml:mrow><mml:mn>2</mml:mn></mml:mrow> </mml:msub> </mml:mrow> <mml:annotation>$$ {F}_2 $$</mml:annotation></mml:semantics> </mml:math> dimension. This high selectivity thus obviates the need for extra filtering elements and pure-shift acquisition schemes that are integrated into existing sequences to facilitate coupling measurements in overcrowded signals. It is therefore anticipated that this sequence, with the ease of implementation and ability to extract coupling values from highly congested spectra, should turn out an important tool for structural and conformational analyses in chemical and biological studies.