Electronic Supplementary Information
Synthesis of chromenoindole derivatives from Robinia pseudoacacia
Lisa Dejon, Hamdoon Mohammed, Peng Du, Claus Jacob and Andreas Speicher*
Experimental section
(1) Isolation of compound 1 from the root of Robinia pseudoacacia
Roots of Robinia pseudoacacia (typically 3.0 kg per batch) were collected freshly from
trees found in the Botanical Garden of Al-Azhar University, Nasr City, Cairo, Egypt.
They were cleaned and air dried for 1-2 weeks, and subsequently grinded down
manually. The powder (usually around 850.0 g) was extracted 5 times with 4 L of 70 %
ethanol. The ethanolic extracts were combined and the solvent was removed at 40°C
under vacuum to dryness. 95.0 g of ethanolic extract were obtained from 3.0 kg of wet
root material. The extract was re-dissolved in H
2
O and the insoluble material was
removed by filtration. The water-soluble fraction (62.0 g) was then washed three times
with petroleum ether to remove any fatty acids and subsequently extracted three times
with ethyl acetate and then with n-butanol, respectively. The solvent was removed at
40°C under vacuum to yield 5.0 g of ethyl acetate extract and 8.5 g of n-butanol extract.
These extracts were dissolved in methanol, combined and applied to silica gel
chromatography (CH
2
Cl
2
:CH
3
OH, 80:20) to yield five fractions, of which three contained
material in excess of 100.0 mg. These fractions were purified further individually by
Sephadex LH-20 chromatography (using methanol as running solvent), ultimately
resulting in five chemically pure compounds. The latter were characterized by one- and
two-dimensional
1
H- and
13
C-NMR and mass spectrometry. Ultimately, these compounds
were identif ied as one known dihydroflavone, 7,4’ -dihydroxy-dihydroflavone (a
compound found in many plants
11
), three chalcons, i.e. 2’-hydroxy-chalcone, 4,2’,4’ -
trihydroxychalcone and 2’ -hydroxy-2,3-dimethoxy-chalcone, and the hitherto unknown
compound 1.
1 1
M.J.C. Falcao, Y.B.M. Pouliquem, M.A.S. Lima, N.V. Gramosa, L.V. Costa-Lotufo, G.C.G.
Militao, C. Pessoa, M.O. De Moraes, E.R. Silveira, J. Nat. Prod. 2005, 68, 423-426.
Electronic Supplementary Material (ESI) for Medicinal Chemistry Communications
This journal is © The Royal Society of Chemistry 2013