核磁共振解析2ppt整理.ppt

2D NMR 图谱 Direct H-C correlations (HSQC)Interaction between H and C atoms through one bond. 1H-1H correlations (COSY) Proton interaction trough three bonds. Long-range 13C-1H correlations (HMBC).Interaction between 13С and 1Н nuclei trough two and three bonds. Nuclear Overhauser Effect (NOE) Interaction between 1H-1 and 1H-2 when they are distanced in the space by r 5 ?. NOE produced NOESY / ROESY 2D NMR spectra. * 结构鉴定: 化合物2-1 H-21a H-21b H-4 H-3 Me-23 Me-20 1H NMR of 2-1 H-2 C-1 C-22 C-9 C-10 C-4 C-21 C-3 C-19 C-20 13C NMR of 2-1 C-2 H-4 H-3 H-2 Me-20 H-18 H-15 H-14 H-13a H-16a H-17a H-6 H-7a 1H,1H-COSY H-11a H-12a HMBC （高场区） C-3 C-7 H-19a H-3 C-2 C-18 Me-20 C-19 H-21a H-21b C-8 C-6 C-5 H-4 检测的是核与核之间的关系 1JC-H correlations C-1 H-1 Spectrum 13C 1H Spectrum 3JH-H correlations H-1 H-2 Spectrum 1Н Spectrum 1Н 适用于重叠峰耦合的判断 HMBC peaks corresponding to 2- and 3-bonds correlations are undistinguishable! С-1 H-i H-k Spectrum 13С Spectrum 1Н r 2D NMR图谱的解析 Organic Structure Analysis, Crews, Rodriguez and Jaspars STRATEGY BASED ON C-H CONNECTIVITY HMBC data is ambiguous (2 or 3 bond correlations – impossible to tell which) Organic Structure Analysis, Crews, Rodriguez and Jaspars STRATEGY BASED ON C-H CONNECTIVITY – HSQC DATA A B C D E F dC a b c d’ d e f label protons in lower case letters Organic Structure Analysis, Crews, Rodriguez and Jaspars STRATEGY BASED ON C-H CONNECTIVITY – HSQC DATA 1.2 CH3 17 F 1.5 CH3 23 E 3.0 2.5 CH2 42 D 4.0 CH 68 C 5.2 CH 124 B 5.5 CH 131 A dH (ppm) DEPT dC (ppm) ATOM Organic Structure Analysis, Crews, Rodriguez and Jaspars STRATEGY BASED ON C-H CONNECTIVITY – HSQC DATA Organic Structure Analysis, Crews, Rodriguez and Jaspars STRATEGY BASED ON C-H CONNECTIVITY – HSQC DATA Organic Structure Analysis, Crews, Rodriguez and Jaspars STRATEGY BASED ON C-H CONNECTIVITY – HSQC DATA Organic Structure Analysis, Crews, Rodriguez and Jaspars STRATEGY BASED ON C-H CONNECTIVITY – HSQ