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化合物1 白色粉末，mp246~248℃， Libermann-Burchard反應(yīng)陽(yáng)性，Ehrlish反應(yīng)顯紅色，推測(cè)為呋甾皂苷，酸水解檢出D-葡萄糖和D-半乳糖，苦杏仁酶解檢出D-葡萄糖，表明D-半乳糖連在苷元上。ESI-MS給出分子離子峰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），為糖上的端基質(zhì)子信號(hào)，其偶合常數(shù)值表明端基碳均為β構(gòu)型，1.32（3H，d），1.03（3H，d），0.98（3H，s），0.88（3H，s）為四個(gè)甲基氫信號(hào)。 13C-NMR（C5D5N，δ，ppm）中，δ105.7、104.8、102.2為糖的端基碳信號(hào)，110.4為一季碳，高場(chǎng)區(qū)除去糖上的碳，有4個(gè)CH3，12個(gè)CH2，7個(gè)CH， 3個(gè)季碳，其苷元含27個(gè)碳，根據(jù)所含碳化學(xué)位移和化學(xué)類型，推測(cè)苷元結(jié)構(gòu)為25（S）-22-羥基-5β呋甾-3β，26-二醇。綜上分析，苷元3位連接糖為β-D-吡喃葡萄糖基（1→2）-β-D-吡喃半乳糖，26位連接β-D-吡喃葡萄糖。 化合物2 淺黃色針晶，mp260~261℃。與FeCl3試劑反應(yīng)呈污綠色，對(duì)HCl-Mg反應(yīng)呈橙紅色。ESI-MS給出離子峰m/z445[M+Na]+，423[M+1] +，表明化合物6的分子量為422。 1H-NMR(DMSO-d6，δ)中， 4.61(1H,d,J=9.8Hz)為1個(gè)葡萄糖端基質(zhì)子，且為β－苷鍵形式存在。另有6.39(1H,s)，6.88(1H,s)和7.40(1H,s)3個(gè)芳香質(zhì)子的信號(hào)。 13C-NMR及DEPT (DMSO-d6，δ)中，在較低場(chǎng)區(qū)，179.1為羰基信號(hào)，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個(gè)信號(hào)提示有2個(gè)苯環(huán)存在。在較高場(chǎng)區(qū)有1個(gè)六碳糖信號(hào)，分別為：81.5、78.8、73.1、70.5、70.2、61.4。 |
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happykeren2008
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3樓2010-10-08 18:52:52
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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 個(gè) 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 個(gè) 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樓2010-10-07 20:04:18
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happykeren2008(金幣+1000, 翻譯EPI+1):謝謝 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樓2010-10-09 09:51:31
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