金钗石斛化学成分的研究(2)

　　3  结果

　　3.1  化合物I

　　白色晶体。 EIMS m/z (%): 240 (M+,100), 225 (49), 197 (45), 139 (18); 1H NMR［(CD3)2CO, 500 MHz］δ: 9.54 (1H, s, 5-OH), 9.08 (1H, s, 2-OH), 7.66 (1H, d, J= 8.8, H-9), 7.53  (1H, d, J= 8.8, H-10), 7.46 (1H, dd, J= 7.6, 7.6, H-7), 7.42 (1H, dd, J= 7.6, 2.0, H-6), 7.13 (1H, dd, J= 7.6, 2.0, H-8), 7.09 (1H, d, J= 2.4, H-1), 7.01 (1H, d, J= 2.4, H-3), 4.17 (3H, s, 4-OMe); 13C NMR ［(CD3)2CO, 125MHz］ δ: 157.8 (s, C-4), 156.8 (s, C-2), 155.7 (s, C-5), 137.5 (s, C-10a), 135.4 (s, C-8a), 130.2 (d, C-7), 127.8 (d, C-9), 127.4 (d, C-10), 121.5 (d, C-8), 120.2 (s, C-4b), 117.4 (d, C-6), 114.0 (s, C-4a), 108.3 (d, C-1),103.1 (d, C-3), 59.1 (q, 4-OMe)。与文献对照, 确定化合物的结构为moscatin［9］。

　　3.2  化合物II

　　浅黄色油状物。 EIMS m/z (%): 274 (M+, 54), 137 (100), 122 (22),107 (9), 94 (16), 77 (11); 1H NMR ［CDCl3, 500 MHz］δ: 6.87 (1H, d, J= 8.0, H-5''), 6.72 (1H, d, J= 8.0, H-6''), 6.65 (1H, s, H-2''), 6.34 (1H, s, H-4'), 6.30 (2H, s, H-2',6'), 3.87 (3H, s, 3''-OCH3),3.78(3H, s, 5'-OCH3), 2.82 (4H, m, 1,2-CH2); 13C NMR ［CDCl3, 125 MHz］δ: 162.1 (s, C-5'), 157.9(s, C-3'), 147.6 (s, C-3''), 145.8 (s,C-1'), 145.0 (s, C- 4''), 135.0 (s, C-1''), 122.3 (d, C-6''), 115.5 (d, C-2''), 112.5 (d, C-5'' ), 109.4 (d, C-2'), 108.1 (d, C-6'), 100.4 (d, C-4'), 57.2 (q, 5'-OCH3), 56.6 (q, 3''-OCH3), 39.6 (t, C-2), 38.5 (t, C-1)。与文献对照, 确定化合物的结构为gigantol［10］。

　　3.3  化合物III

　　浅黄色油状物，EIMS m/z (%): 244 (M+, 30), 137 (100), 107 (43), 77 (8); 1H NMR ［(CD3)2CO, 500 MHz］δ: 7.12 (1H, dd, J= 7.7, 7.7, H-3''), 6.73 (1H, d, J= 7.7, H-2''), 6.67 (1H, d, J=7.4, H-4''), 6.33 (1H, s, H-6''), 6.35 (1H, s, H-4'), 6.26 (2H, s, H-2',6'), 3.73 (3H, s, 5'-OCH3), 2.82 (4H, m, 1,2-CH2); 13C NMR (CD3COCD3, 125 MHz) δ: 162.0 (s, C-5'), 159.4 (s, C-3'), 158.3 (s, C-5''), 145.1 (s, C-1'), 144.3 (s, C-1''), 130.0 (d, C-3''), 120.4(d, C-2''), 116.2 (s, C-6''), 113.7 (s, C-4''), 108.9 (s, C-2'), 106.3 (s, C-6'), 99.8 (s,C-4'), 55.3 (q, 5'-OCH3), 38.6 (t, C-1), 38.2 (t, C-2)。与文献对照, 确定化合物的结构为batatasin III［10］。

　　3.4  化合物IV

　　白色针状晶体。mp 138～140 ℃ (EtOAc). EIMS m/z (rel int.) 412 ［M+］, (100), 369 (16), 351 (55), 300 (45), 271 (70), 255 (93), 213 (30), 145 (31), 91 (44); 1H NMR (CDCl3, 500Mz) δ: 0.70 (3H, s, H-18), 0.79 (3H, d, J = 6.5, H-27), 0.80 (3H, t, J = 7.5, H-29), 0.84 (3H, d, J = 6.5, H-26), 1.01 (3H, s, H-19), 1.02 (3H, d, J = 6.5, H-21), 3.50 (1H, m, H-3), 5.02 (1H, dd, J = 15, 8.5, H-23), 5.15 (1H, dd, J = 15, 8.5, H-22), 5.35 (1H, br d, H-6). 13C NMR (CDCl3, 125 Mz) δ: 12.0 (q, C-18), 12.2 (q, C-29), 19.0 (q, C-27), 19.4 (q, C-19), 21.1 (t, C-26), 21.1 (q, C-21), 21.2 (t, C-11), 24.4 (t, C-15), 25.4 (q, C-28), 28.9 (t, C-16), 29.7 (d, C-25), 31.7 (t, C-2), 31.9 (t, C-7), 31.9 (d, C-8), 36.5 (s, C-10), 37.3 (t, C-1), 39.7 (t, C-12), 40.5 (d, C-20), 42.2 (d, C-13), 42.3 (t, C-4), 50.2 (d, C-9), 51.2 (d, C-24), 56.0 (d, C-17), 56.9 (d, C-14), 71.8 (d, C-3), 121.7 (d, C-6), 129.3 (d, C-23), 138.3 (d, C-22), 140.7 (s, C-5)。易溶于氯仿。15%H2SO4乙醇溶液显色为紫红色，与豆甾醇标准品进行TLC对照，在多种溶剂系统中Rf值均相同。且1H NMR, 13C NMR数据与豆甾醇一致，确定其为豆甾醇［11］。

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