核磁共振波谱分析ppt整理.ppt

* * * * * * * * * * * Writing a NMR Report Writing a NMR Report A doublet, J = ? Hz Writing a NMR Report 2,3-Dihydroxy-5-iodo-benzoic acid methyl ester 3. To an oven-dried round bottom flask charged with 2,2-dihydoxybenzoic acid methyl ester (1.1 g, 100 mol%, 3.6 mmol) was added BBr3 solution in DCM (1M, 200 mol%, 7.2 mL) at -78 oC under argon. The reaction was allowed to stir for 30 min, and was warmed to rt for additional 20 min. The reaction mixture was quenched with ice water (30 mL), and extracted with DCM two times (2×20 mL). The combined organic layer was dried (MgSO4) and filtered. The crude material was dried onto silica gel under reduced pressure. Flash column chromatography (SiO2: 3% ethyl acetate in hexanes) gave the title compound as a white solid (0.70 g, 2.38 mmol, 67% yield). 1H NMR (400 MHz, CDCl3): ? 10.72 (s, 1H), 7.54 (s, 1H), 7.53 (s, 1H), 5.49 (s, 1H), 3.80 (s, 3H). 13C NMR (100 MHz, CDCl3): ? 169.2, 148.5, 145.6, 128.8, 128.0, 113.7, 79.7, 52.5. HRMS (ESI): m/z [M+H]+ found 294.944, calcd 294.947 for C8H8IO4. MP = 133-134 oC. Writing a NMR Report Writing a NMR Report 400 MHz, CDCl3: 5.32 (t, J = 9.6 Hz, 1H; H3), 5.21 (t, J = 9.6 Hz, 1H; H4), 5.07 (t, J = 9.6 Hz, 1H; H2), Writing a NMR Report 100 MHz, CDCl3: (2S, 3S, 4R, 5R, 6R)- 4-(3,4,5-Triacetoxy-6-acetoxymethyl-tetrahydro-pyran-2-yl)-benzoic acid methyl ester. 1H NMR (400 MHz, CDCl3): ? 7.99 (d, J = 8.0 Hz, 2H), 7.39 (d, J = 8.0 Hz, 2H), 5.32 (t, J = 9.6 Hz, 1H; H3), 5.21 (t, J = 9.6 Hz, 1H; H4), 5.07 (t, J = 9.6 Hz, 1H; H2), 4.43 (d, J = 10.0 Hz, 1H; H1), 4.28 (dd, J = 12.4 and 4.8 Hz, 1H; H1), 4.15 (dd, J = 12.4 and 2.4 Hz, 1H; H7), 3.88 (s, 3H), 3.83 (ddd, J = 10.0, 4.8 and 2.4 Hz, 1H; H5), 2.07 (s, 3H), 2.04 (s, 3H), 1.97 (s, 3H), 1.79 (s, 3H). 13C NMR (100 MHz, CDCl3): ? 170.6, 170.3, 169.4, 168.7, 166.6, 141.2, 130.7, 129.7, 127.1, 79.7, 76.3, 74.1, 72.6, 68.6, 62.3, 52.1, 20.7, 20.6, 20.3. Writing a NMR Report 核磁共振谱解析实例 二. 未知化合物1H NMR谱图解析实例 例4：某化合物的分子式为C6H10O3，其核磁共振谱见图。试确定该化合物结构。