【摘要】 牙节(Dregea volubili fL.)Benth)系萝藦科南山藤属植物,从其根的甲醇提取处理后所得粗甙水解物,分离到两个α-甲基双糖甙Ⅰ,Ⅱ(Ⅰ,Ⅱ得率分别为0.016%和0.0097%)。Ⅰ,Ⅱ及其乙酰化物经各种波谱分析并比较物理性质,推证为:Ⅰ,α-甲基-茯苓双糖甙;Ⅱ,α-甲基-{3-O-甲基-6-去氧-D-阿洛糖(1→4)D-橄榄糖]-甙。Ⅱ系首次报道,命名为α-甲基-牙节双糖甙。更多还原

【Abstract】 From the hydrolysate of the crude glycosides from the roots,of Dregea volubilis （L） Benth in Dehong,Yunnan,two α-methyl biosides I and Ⅱ（yields:0.016% and 0.0097%,respectively） were isolated by silica gel column chromatography.Their chemical structures were established by interpretation of MS,IR,¹H,¹³C-NMR,and gas chromatographic analysis of their degradatioh products,and comparison of the physical properties of Ⅰ,Ⅱ and their acetates which were reported in literatures as follows:α-methyl-pachybioside for I,and α-methyl-[3-O-methyl-6-deoxy-D-allose (→D-olivoside] forⅠ.Ⅱnamed α-methyl-dredehongbioside,is reported for the first time. Ⅱ,α-methy-dredehongbioside,coloriess needles （from MeOH）,bitter,mp.184— 186℃,[a]_D²²+74.5^c=0.52,MeOH.Anal.Cald（%） for C₁4H₂6O₈:C52.17,H8.07; Found;C52.23,H8.22.IRv_max^KBr:3370,1443,1419,1375,1268,1218,1168,1127,1060 cm^-1.MS（m/e,%）:322（M⁺,3）,291（M⁺-OCH₃,15）,273（M⁺-OCH₃-H,O,12）,258, 246,232,222,159,145,141,128,95,87,85,74 （base peak,100）,59.H NMRB （CDCI₃）:4.73（1H,dd,J=4.0Hz,J=1.5Hz,C-1-H）,4.55（1H,d,J=8.0Hz, C-I′-H）,3.79（1H,dd,J=3.0Hz,J=3.0Hz,C-3′-H）,3.00（1H,dd,J=9.0Hz, J=9.0Hz,C-4-H）,2.22（IH,m,C-2-Ha）,1.60（IH,m,C-2-He）,1.33（3H,d, J=6.0Hz,C-5-CH,）,1.31（3H,d,J=6.5Hz,C-5′-CH,）,3.68（3H,s,C-3′-OCH）, 3.31（3H,s,C-1-OCH）.¹³C NMR data were seen in Table 1. Ⅳ,tri-acetyl-α-methyl-dredehongbioside,colorless granular （from MeOH）, rap.135—137℃,[α]D₂2+88.2°（c=0.50,MeOH）.MS（m/e,%）:488（M₊,2）,388 （M+-HOAc,2）,357（M₊-OCH₃-HOAc,33）,288,187,127,116,85,74,59,43（base peak,100）.¹H NMR δ（CDCl₃）:5.25（1H,ddd,J=11.0Hz,J=9.0Hz,J=5.5Hz, C-3-H）,4.86（1H,d,J=8.0Hz,C-1′-H）,4.69（1H,dd,J=4.0Hz,J=1.5Hz, C-1-H）,4.58（1H,m,C-2′-H）,3.94（1H,dd,J=3.0Hz,J=3.0Hz,C-3′-H）,3.64（IH, m,C-5-H）,3.22（1H,dd,J=9.SHz,J=8.5Hz,C-4-H₃）,2.30（1H,m,C-2-Ha）, 1.67（1H,m,C-2-He）,1.31（3H,d,J=6.5Hz,C-5-CH₃）,1.17（3H,d,J=6.0Hz, C-5-CH3）,3.47（3H,s,C-3′-OCH₃）,3.30（3H,s,C-1-OCH₃）,2.10（6H,s,C-2′, C-4′-CCH₃）,2.03（3H,s,C-3-CCH₃）.更多还原