化合物5 红棕色胶状物;ESI-MS m/z 258 -。铁皮1H-NMR (CD3OD,石斛400 MHz) δ: 6.22 (1H,联苄类化 d, J = 1.8 Hz, H-2),6.38 (1H,学成 d, J = 1.7 Hz, H-6),6.76 (1H,研究 d, J = 1.6 Hz, H-2'),6.73 (1H,铁皮 dd, J = 7.8, 1.6 Hz, H-4'),6.97 (1H,石斛 t, J = 7.6 Hz, H-5'),6.74 (1H,联苄类化 d, J = 7.4 Hz, H-6'),2.66 (2H,学成 m, H-α),2.72 (2H,研究 m, H-α'),3.69 (3H,铁皮 s, 3-OMe);13C-NMR (CD3OD,100 MHz) δ: 134.1 (C-1),石斛105.0 (C-2),联苄类化149.2 (C-3),学成132.9 (C-4),研究146.1 (C-5),110.0 (C-6),144.6 (C-1'),116.5 (C-2'),159.0 (C-3'),113.6 (C-4'),130.4 (C-5'),120.9 (C-6'),38.8 (C-α),39.0 (C-α'),56.5 (3-OMe)。参考文献报道,鉴定化合物为dendrosinen B。 化合物6 红色胶状物;ESI-MS m/z 258 -。1H-NMR (CD3OD,400 MHz) δ: 6.22 (1H, d, J = 1.7 Hz, H-2),6.29 (1H, d, J = 1.6 Hz, H-6),6.94 (2H, d, J = 8.4 Hz, H-2', 6'),6.68 (2H, d, J = 8.4 Hz, H-3', 5'),2.67 (2H, m, H-α),2.74 (2H, m, H-α'),3.74 (3H, s, 5-OMe);13C-NMR (CD3OD,100 MHz) δ: 133.2 (C-1),110.1 (C-2),146.1 (C-3),134.3 (C-4),149.5 (C-5),105.2 (C-6),146.3 (C-1'),130.6 (C-2', 6'),116.1 (C-3', 5'),156.4 (C-4'),38.5 (C-α),39.4 (C-α'),56.6 (5-OMe)。参考文献报道,鉴定化合物为3,4,4'-三羟基-5-甲氧基联苄。 化合物7 棕色胶状物;ESI-MS m/z 272 -。1H-NMR (CD3Cl3,400 MHz) δ: 6.46 (1H, s, H-2),6.24 (1H, s, H-6),6.67 (2H, m, H-2', 4'),7.14 (1H, t, J = 7.6 Hz, H-5'),6.76 (1H, d, J = 7.5 Hz, H-6'),2.79 (4H, m, H-α, α'),3.86 (3H, s, 4-OMe),3.80 (3H, s, 5-OMe);13C-NMR (CD3Cl3,100 MHz) δ: 143.5 (C-1),108.2 (C-2),149.0 (C-3),138.3 (C-4),152.3 (C-5),104.7 (C-6),133.7 (C-1'),115.6 (C-2'),155.8 (C-3'),113.0 (C-4'),129.6 (C-5'),120.9 (C-6'),37.8 (C-α),37.6 (C-α'),61.1 (4-OMe),55.8 (5-OMe)。参考文献报道,鉴定化合物为3,3'-二羟基-4,5-二甲氧基联苄。 化合物8 无色针晶;ESI-MS m/z 242 -。1H-NMR (CD3OD,400 MHz) δ: 6.23 (1H, s, H-2),6.18 (1H, d, J = 2.0 Hz, H-4),6.20 (1H, s, H-6),6.97 (2H, d, J = 8.4 Hz, H-2', 6'),6.68(2H, d, J = 8.4 Hz, H-3', 5'),2.73 (4H, m, H-α, α'),3.69 (3H, s, 5-OMe);13C-NMR (CD3OD,100 MHz) δ: 145.7 (C-1),109.3 (C-2),159.3 (C-3),100.0 (C-4),162.2 (C-5),106.8 (C-6),134.2 (C-1'),130.5 (C-2', 6'),116.1 (C-3', 5'),156.4 (C-4'),38.1 (C-α),39.7 (C-α'),55.7 (5-OMe)。参考文献报道,鉴定化合物为3,4'-二羟基-5-甲氧基联苄。 化合物9 白色针晶;ESI-MS m/z 304 +。1H-NMR (CD3OD,400 MHz) δ: 6.60 (1H, d, J = 1.9 Hz, H-2),6.67 (1H, dd, J = 14.0, 2.2 Hz, H-6),6.37 (2H, s, H-2', 6'),6.82 (1H, d, J = 8.7 Hz, H-5'),2.81 (4H, s, H-α, α'),3.83 (3H, s, 3'-OMe),3.84 (6H, s, 3, 5-OMe);13C-NMR (CD3OD,100 MHz) δ: 132.9 (C-1),111.3 (C-2),143.8 (C-3),146.3 (C-4),146.9 (C-5),121.2 (C-6),133.86 (C-1'),105.3 (C-2'),146.9 (C-3'),133.7 (C-4'),114.2 (C-5'),105.3 (C-6'),37.5 (C-α),39.0 (C-α'),55.93 (3'-OMe),56.28 (3, 5-OMe)。参考文献报道,鉴定化合物为杓唇石斛素。 化合物10 淡黄色油状液体;ESI-MS m/z 273 -。1H-NMR (CD3Cl3,400 MHz) δ: 6.24 (2H, d, J = 1.9 Hz, H-2, 6),6.30 (1H, t, J = 1.9 Hz, H-4),6.61 (1H, d, J = 1.9 Hz, H-2'),6.83 (1H, d, J = 8.0 Hz, H-5'),6.67 (1H, dd, J = 8.0, 1.9 Hz, H-6'),2.81 (4H, m, H-α, α'),3.74 (3H, s, 3-OMe),3.84 (3H, s, 3'-OMe);13C-NMR (CD3Cl3,100 MHz) δ: 144.6 (C-1),106.8 (C-2),160.8 (C-3),99.0 (C-4),156.6 (C-5),108.2 (C-6),133.7 (C-1'),111.2 (C-2'),146.1 (C-3'),143.7 (C-4'),114.2 (C-5'),121.1 (C-6'),38.5 (C-α),37.4 (C-α'),55.3 (3-OMe),55.8 (3'-OMe)。参考文献报道,鉴定化合物为石斛酚。 化合物11 无色针晶;ESI-MS m/z 274 +。1H-NMR (CD3OD,400 MHz) δ: 6.36 (2H, s, H-2, 6),6.94 (2H, d, J = 8.4 Hz, H-2', 6'),6.67 (2H, d, J = 8.4 Hz, H-3', 5'),2.76 (2H, s, H-α, α'),3.76 (6H, s, 3, 5-OMe);13C-NMR (CD3OD,100 MHz) δ: 134.2 (C-1),107.0 (C-2,6),149.1 (C-3, 5),130.7 (C-4, 1'),130.6 (C-2', 6'),116.1 (C-3', 5'),156.5 (C-4'),39.7 (C-α),38.6 (C-α'),56.8 (3, 5-OMe)。参考文献报道,鉴定化合物为4,4'-二羟基-3,5-二甲氧基联苄。 化合物12 白色固体;ESI-MS m/z 258 -。1H-NMR (CD3OD,400 MHz) δ: 6.12 (2H, d, J = 2.2 Hz, H-2, 6),6.08 (1H, t, J = 2.2 Hz, H-4),6.66 (1H, d, J = 1.8 Hz, H-2'),6.68 (1H, d, J = 8.0 Hz, H-5'),6.60 (1H, dd, J = 8.0, 1.9 Hz, H-6'),2.69 (2H, m, H-α),2.77 (2H, m, H-α'),3.78 (3H, s, 3'-OMe);13C-NMR (CD3OD,100 MHz) δ: 145.7 (C-1),108.3 (C-2,6),159.5 (C-3,5),101.3 (C-4),134.9 (C-1'),113.5 (C-2'),148.8 (C-3'),145.7 (C-4'),116.1 (C-5'),122.0 (C-6'),39.7 (C-α),38.6 (C-α'),56.4 (3'-OMe)。参考文献报道,鉴定化合物为3,4',5-三羟基-3'-甲氧基联苄。 化合物13 白色无定形粉末;ESI-MS m/z 287 -。1H-NMR (CD3Cl3,400 MHz) δ: 6.24 (2H, d, J = 1.9 Hz, H-2, 6),6.31 (1H, t, J = 1.9 Hz, H-4),6.65 (1H, d, J = 1.9 Hz, H-2'),6.78 (1H, d, J = 8.1 Hz, H-5'),6.71 (1H, dd, J = 8.0, 1.9 Hz, H-6'),2.81 (4H, m, H-α, α'),3.74 (3H, s, 3-OMe),3.85 (3H, s, 3'-OMe),3.83 (3H, s, 4'-OMe);13C-NMR (CD3Cl3,100 MHz) δ: 146.1 (C-1),105.7 (C-2),159.7 (C-3),97.8 (C-4),155.5 (C-5),106.8 (C-6),133.2 (C-1'),110.1 (C-2'),147.6 (C-3'),143.4 (C-4'),110.7 (C-5'),119.1 (C-6'),37.1 (C-α),36.0 (C-α'),54.8 (3-OMe),54.7 (3'-OMe),54.1 (4'-OMe)。参考文献报道,鉴定化合物为3-O-methylgigantol。 化合物14 白色无定形粉末;ESI-MS m/z 467 -。1H-NMR (CD3OD,400 MHz) δ: 6.43 (1H, d, J = 1.8 Hz, H-2),6.37 (1H, d, J = 1.8 Hz, H-6),6.96 (2H, m, H-2', 6'),6.68 (2H, d, J = 2.0 Hz, H-3', 5'),6.66 (2H, br s, H-2'', 6''),5.18 (1H, d, J = 2.5 Hz, H-7''),3.97 (1H, s, H-8''),3.56 (1H, dd, J = 12.1, 8.2 Hz, H-9''a),3.86 (1H, s, H-9''b),2.77 (4H, s, H-α, α'),3.79 (9H, s, 5, 3'', 5''-OMe);13C-NMR (CD3OD,100 MHz) δ: 136.2 (C-1),111.0 (C-2),145.0 (C-3),131.3 (C-4),149.5 (C-5),107.0 (C-6),134.1 (C-1'),130.7 (C-2',6'),116.1 (C-3',5'),156.6 (C-4'),128.7 (C-1''),105.0 (C-2'',6''),149.5 (C-3'',5''),136.2 (C-4''),77.1 (C-7''),79.1 (C-8''),60.2 (C-9''),39.3 (C-α),38.3 (C-α'),56.9 (5, 3'', 5''-OMe)。参考文献报道,鉴定化合物为dendrocandin U。 化合物15 黄色胶状物;ESI-MS m/z 436 -。1H-NMR (CD3OD,400 MHz) δ: 6.28 (1H, d, J = 1.7 Hz, H-2),6.24 (1H, d, J = 1.7 Hz, H-6),6.84 (2H, d, J = 8.4 Hz, H-2', 6'),6.69 (2H, d, J = 8.4 Hz, H-3', 5'),6.64 (1H, d, J = 1.8 Hz, H-2''),6.57 (1H, d, J = 1.9 Hz, H-5''),6.58 (1H, dd, J = 8.0, 1.9 Hz, H-6''),4.61 (1H, s, H-7''),3.77 (1H, m, H-8''),3.76 (2H, d, J = 1.2 Hz, H-9''b),2.78 (4H, s, H-α, α'),3.77 (6H, s, 5, 3''-OMe);13C-NMR (CD3OD,100 MHz) δ: 135.4 (C-1),110.5 (C-2),145.7 (C-3),132.3 (C-4),149.1 (C-5),107.1 (C-6),134.2 (C-1'),130.7 (C-2', 6'),116.1 (C-3', 5'),156.6 (C-4'),129.6 (C-1''),112.1 (C-2''),122.2 (C-3'),148.2 (C-4''),116.0 (C-5''),121.7 (C-6''),77.4 (C-7''),79.7 (C-8''),62.0 (C-9''),39.6 (C-α),39.1 (C-α'),56.8 (5-OMe),56.5 (3''-OMe)。参考文献报道,鉴定化合物为dendrocandin N。 声明:本文所用图片、文字来源《中国中药杂志》,版权归原作者所有。如涉及作品内容、版权等问题,请与本网联系删除。
相关链接:化合物,甲氧基联苄,二羟基 |
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