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化合物1 白色粉末，mp246~248℃， Libermann-Burchard反应阳性，Ehrlish反应显红色，推测为呋甾皂苷，酸水解检出D-葡萄糖和D-半乳糖，苦杏仁酶解检出D-葡萄糖，表明D-半乳糖连在苷元上。ESI-MS给出分子离子峰920。 1H-NMR（C5D5N，δ，ppm）中， 5.28（1H，d，J=7Hz）、4.91（1H，d，J=8Hz）、4.80（1H，d，J=8Hz），为糖上的端基质子信号，其偶合常数值表明端基碳均为β构型，1.32（3H，d），1.03（3H，d），0.98（3H，s），0.88（3H，s）为四个甲基氢信号。 13C-NMR（C5D5N，δ，ppm）中，δ105.7、104.8、102.2为糖的端基碳信号，110.4为一季碳，高场区除去糖上的碳，有4个CH3，12个CH2，7个CH， 3个季碳，其苷元含27个碳，根据所含碳化学位移和化学类型，推测苷元结构为25（S）-22-羟基-5β呋甾-3β，26-二醇。综上分析，苷元3位连接糖为β-D-吡喃葡萄糖基（1→2）-β-D-吡喃半乳糖，26位连接β-D-吡喃葡萄糖。 化合物2 浅黄色针晶，mp260~261℃。与FeCl3试剂反应呈污绿色，对HCl-Mg反应呈橙红色。ESI-MS给出离子峰m/z445[M+Na]+，423[M+1] +，表明化合物6的分子量为422。 1H-NMR(DMSO-d6，δ)中， 4.61(1H,d,J=9.8Hz)为1个葡萄糖端基质子，且为β－苷键形式存在。另有6.39(1H,s)，6.88(1H,s)和7.40(1H,s)3个芳香质子的信号。 13C-NMR及DEPT (DMSO-d6，δ)中，在较低场区，179.1为羰基信号，163.6、161.4、156.3、153.8、150.8、143.6、111.8、108.1、107.5、102.6、101.3、93.4的12个信号提示有2个苯环存在。在较高场区有1个六碳糖信号，分别为：81.5、78.8、73.1、70.5、70.2、61.4。 |
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White powder Compound 1 , mp246 ~ 248 ℃, Libermann-Burchard-positive, Ehrlish reaction was red, presumably furostanol saponins, acid hydrolysis detected D-glucose and D-galactose, D-amygdalin enzymatic detection of glucose, D-galactose showed that even on the aglycone. ESI-MS gives the molecular ion peak 920. 1H-NMR (C5D5N, δ, ppm) in, 5.28 (1H, d, J = 7Hz), 4.91 (1H, d, J = 8Hz), 4.80 (1H, d, J = 8Hz), for the sugar on the side matrix sub-signals, the coupling constant values that were β-side configuration of carbon, 1.32 (3H, d), 1.03 (3H, d), 0.98 (3H, s), 0.88 (3H, s) for the four methyl H signal. 13C-NMR (C5D5N, δ, ppm) in, δ105.7, 104.8,102.2 end groups for the sugar carbon signals, 110.4 for the season, carbon, high-field region of the carbon on the removal of sugar, 4 CH3, 12 个 CH2, 7 CH, 3 quarters of carbon, with 27 of its aglycone carbon, according to the chemical shift and chemical types of carbon, suggesting that aglycone structure of 25 (S) -22 - hydroxy-5β furostanol-3β, 26 - II alcohol. The foregoing analysis, aglycone 3 connections sugar β-D-glucopyranosyl (1 → 2)-β-D-pyran-galactose, 26 connecting β-D-glucopyranose. Light yellow needle crystal of compound 2, mp260 ~ 261 ℃. FeCl3 reagent was dirty and green, on the HCl-Mg reaction was orange red. ESI-MS shows ions m/z445 [M + Na] +, 423 [M +1] +, showed that the molecular weight of compounds 6, 422. 1H-NMR (DMSO-d6, δ) in, 4.61 (1H, d, J = 9.8Hz) glucose as a substrate sub-terminal, and for the β-glucoside bond form. Another 6.39 (1H, s), 6.88 (1H, s) and 7.40 (1H, s) 3 个 aromatic proton signals. 13C-NMR and DEPT (DMSO-d6, δ), in the low field region, 179.1 for the carbonyl signal, 163.6,161.4,156.3,153.8,150.8,143.6,111.8,108.1,107.5,102.6,101.3,93.4 12 a signal suggestive of two benzene rings exist. In the high field region have a six-carbon sugar signal, namely: 81.5,78.8,73.1,70.5,70.2,61.4. |
2楼2010-10-07 20:04:18
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3楼2010-10-08 18:52:52
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4楼2010-10-08 19:27:37
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happykeren2008(金币+1000, 翻译EPI+1):谢谢 2010-10-10 20:46:36
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Compound 1 Compound 1, white powered, melting point 246~248℃, which exhibits positive in Libermann-Burchard reaction and red in Ehrlish reaction was supposed to be furostanol saponins. Detection of D-glucose and D-galactose with acid hydrolysis and D-glucose with emulsin enzymolysis indicates that D-galactose was connected to the aglycone. ESI-MS manifests molecularion peak at 920. For 1H-NMR test (C5D5N, δ, ppm), anomeric proton signal of carbohydrate are 5.28(1H, d, J=7Hz), 4.91(1H, d, J=8Hz) and 4.80(1H, d, J=8Hz), while coupling constant values of compound 1 indicates the β-configuration of all anomeric carbons. 1.32(3H, d), 1.03(3H, d), 0.98(3H, s) and 0.88(3H, s) are four methyl hydrogen signals. For 13C-NMR test (C5D5N, δ, ppm), δ105.7, 104.8, 102.2 and 110.4 are anomeric carbons signals of carbohydrate and 110.4 represents C-1. Excluding carbon from carbohydrate in upfield region, there are four CH3，twelve CH2，seven CH and three quaternary carbons. Aglycone of compound 1 contains twenty-seven carbons. In accordance with chemical shift and type of carbons in the aglycone, it is suspected that the structure of aglycone is 25(s)-22-hydroxy-5β furostanol-3β, 26-glycol. Based upon the analysis listed above, carbohydrate connected to C3 of aglycone is β-D-glucopyranosyl(1→2)-β-D-galactopyranose and C26 of aglycone is β-D-glucopyranose. Compound 2 Compound 2, which is buff acicular crystal, exhibits dirty green in reaction with FeCl3 and almon pink in HCL-Mg reaction. ESI-MS manifests molecularion peak at m/z445 [M+Na]+, 423[M+1]+ indicates molecular mass of compound 6 is 422. For 1H-NMR test (DMSO-d6, δ), 4.61(1H, d, J=9.8Hz) represents one glucose anomeric proton which exists as β-glucoside bond. In addition, 6.39(1H, s), 6.88(1H, s) and 7.40(1H, s) are three aromatic protons. For 13C-NMR and DEPT (DMSO-d6, δ) test, 179.1 is carbonyl signal in downfield region and twelve signals of 163.6, 161.4, 156.3, 153.8, 150.8, 143.6, 111.8, 108.1, 107.5, 102.6, 101.3, and 93.4 indicate the compound includes two benzene rings. 81.5, 78.8, 73.1, 70.5, 70.2 and 61.4 represents a hexose signal in upfield region. |
5楼2010-10-09 09:51:31
