Division of Agriculture and Agricultural Life Sciences, The University of Tokyo, Yayoi, Bunkyo-ku, Tokyo, 113-8657, Japan.
Magn Reson Chem. 2014 Jan-Feb;52(1-2):27-31. doi: 10.1002/mrc.4032. Epub 2013 Nov 26.
Natural products often possess various spin systems consisting of a methine group directly bonded to a methyl group (e.g. -CHa-CHb(CH3)-CHc-). The methine proton Hb splits into a broadened multiplet by coupling with several vicinal protons, rendering analysis difficult of (n)JC-H with respect to Hb in the J-resolved HMBC-1. In purpose of the reliable and easy measurements of (n)JC-H and (n)JH-H in the aforesaid spin system, we have developed a new technique, named BASHD-J-resolved-HMBC. This method incorporates band selective homo decoupled pulse and J-scaling pulse into HMBC. In this method, high resolution cross peaks can be observed along the F1 axis by J-scaling pulse, and band selective homo decoupled pulse simplified multiplet signals. Determinations of (n)JC-H and (n)JH-H of multiplet signals can easily be performed using the proposed pulse sequence.
天然产物通常具有各种由直接与甲基(例如-CHa-CHb(CH3)-CHc-)相连的亚甲基组成的自旋系统。亚甲基质子 Hb 通过与几个相邻质子的偶合分裂为一个展宽的多重峰,使得(n)JC-H 相对于 Hb 在 J 分辨 HMBC-1 中的分析变得困难。为了可靠且易于测量上述自旋系统中的(n)JC-H 和(n)JH-H,我们开发了一种新的技术,称为 BASHD-J 分辨 HMBC。该方法将带选择性同核去耦脉冲和 J 标度脉冲结合到 HMBC 中。在该方法中,通过 J 标度脉冲可以在 F1 轴上观察到高分辨率的交叉峰,并且带选择性同核去耦脉冲简化了多重峰信号。可以使用所提出的脉冲序列轻松确定多重峰信号的(n)JC-H 和(n)JH-H。