Experimental access to HSQC spectra decoupled in all frequency dimensions.
A new operator called RESET "Reducing nuclEar Spin multiplicitiEs to singuleTs" is presented to acquire broadband proton decoupled proton spectra in one and two dimensions. Basically, the homonuclear decoupling is achieved through the application of bilinear rotation pulses and delays. A [BIRD](r,x) pulse building block is used to selectively invert all proton magnetization remotely attached to (13)C isotopes, which is equivalent to a scalar J decoupling of the protons directly attached to (13)C from all other protons in the spin system. In conjunction with an appropriate data processing technique pure shift proton spectra are obtained. For this purpose, the concept of constant time acquisition in the observe dimension is exploited. Both ideas were merged together producing superior HSQC based pseudo 3D pulse sequences. The resulting HSQC spectra show cross peaks with collapsed multiplet structures and singlet responses for the proton chemical shift frequencies. An unambiguous assignment of signals from overcrowded spectra becomes much easier. Finally, the recently introduced SHARC technique is exploited to enhance the capability of the scalar J decoupling method. A significant reduction of the total measurement time is achieved. The time is saved by reducing the number of (13)C chemical shift evolution increments and working with superimposed narrow spectral bandwidths in the (13)C indirect domain.
Sakhaii
Peyman
P
Sanofi-Aventis Deutschland GmbH, Process Development Chemistry, PDC SPS (Structure Elucidation/Project & Production Support), Industriepark Hoechst, Frankfurt/Main, Germany. Peyman.Sakhaii@sanofi-aventis.com
Haase
Burkhard
B
Bermel
Wolfgang
W
D000465:Algorithms; D003198:Computer Simulation; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008956:Models, Chemical; D011522:Protons
D011522:Protons