1) Institute of Petroleum Chemistry and Catalysis, Academy of Sciences of the Republic of Bashkortostan and Ufa
Scientific Center, Russian Academy of Sciences; 2) N. D. Zelinskii Institute of Organic Chemistry, Russian Academy of
Sciences. Translated from Khimiya Prirodnykh Soedinenii, No. 3, pp. 223-225, May-June, 2003. Original article submitted
May 10, 2003.
0009-3130/03/3903-0285$25.00
©
2003 Plenum Publishing Corporation
285
RO
1
3
5
7
9
10
11
13
15
17
30
29 19
21
28
27
24
23
A
B
C
26
D
E
1a: R = Ac;
1b: R = H
25
Chemistry of Natural Compounds, Vol. 39, No. 3, 2003
PMR AND
13
C NMR SPECTRA OF BIOLOGICALLY
ACTIVE COMPOUNDS. XII.* TARAXASTEROL AND
ITS ACETATE FROM THE AERIAL
PART OF Onopordum acanthium
L. M. Khalilov,
1
A. Z. Khalilova,
1
E. R. Shakurova,
1
UDC 547.92
I. F. Nuriev,
1
V. V. Kachala,
2
A. S. Shashkov,
2
and U. M. Dzhemilev
1
Crystalline taraxasterol and its acetate were isolated for the first time from Onopordum acanthium. Two-
dimensional COSY, HSQC, and HMBC NMR experiments were carried out for complete assignment of signals
in the PMR and
13
C NMR. Chemical shifts of stereochemically important methyl C atoms C-28 and C-29
were measured.
Key words: Onopordum acanthium L., two-dimensional spectrum, PMR,
13
C NMR, HSQC, HMBC, COSY, TOCSY,
ROESY spectra.
Scotch thistle (Onopordum acanthium L., Asteraceae) is a biennial herbaceous plant. It has application in medical
practice as a bactericide, cardiotonic, and hemostatic agent and is used against hypotonicity [2-4]. The lactones arctiopicrin
and onopordopicrin [2] were isolated from leaves of Scotch thistle; alcohols lupeol and amyrin as their acetates [5] from seeds.
Our goal was to isolate and establish the structure of new biologically active terpenoids from Onopordum acanthium
using PMR and
13
C NMR spectra.
The aerial part of Onopordum acanthium was investigated for the presence of biologically active compounds.
Extraction by CHCl
3
and chromatography over a silica-gel column using ethylacetate:hexane afforded pure crystalline
compounds. IR spectra and
13
C NMR spectra of one of the compounds were similar to those of taraxasteryl acetate 1a [6, 7].
However, the melting point of the isolated compound (232-234°C) differed substantially from the literature value (256-257°C
[8]).
Therefore, we investigated the NMR spectra of the isolated compounds. Table 1 lists the principal PMR and
13
C NMR
spectral properties for taraxasterol (1b) and its acetate (1a).
______
*For No. XI, see [1]. Work supported by RFBR Grants Nos. 00-03-40132, 01-04-49274, 02-03-97901.