Alkaloids of a new type from Elaeocarpus polydactylus Schl. (family elaeocarpaceae)

Chemical Communications (London)
1968.0

Abstract

No structural information regarding alkaloids of the family Elaeocarpaceae has previously been reported. We now report that two new alkaloids, elaeocarpine, C₁₇H₁₇NO₃, m.p. 81-82°, [α]ᴅ ca. +0.6° in CHCl₃, and an isomer, isoelaeocarpine, C₁₇H₁₇NO₃, m.p. 51-52°, [α]ᴅ ca. +0.4° in CHCl₃, isolated from the leaves of a New Guinea species Elaeocarpus polydactylus Schl., are the first members of a new class of indolizidine alkaloids. The complete stereochemistry of elaeocarpine (I) has been established by an X-ray crystal structure analysis of elaeocarpine hydrobromide which crystallizes in the triclinic system with two formula units in a unit cell of dimensions a = 12.46 Å, b = 7.38 Å, and c = 8.05 Å, α = 96.1°, β = 92.8° and γ = 94.0°; the N(z) versus z test clearly shows the space group to be Pī, indicating essentially racemic crystals, and the electron-density map (based on bromine atom co-ordinates from the Patterson function) reveals the positions of all C, N, and O atoms. The isomeric alkaloid isoelaeocarpine (II) is closely related to elaeocarpine, as shown by their interconversion in methanolic potassium hydroxide solution at room temperature. Both alkaloids exhibit carbonyl absorption bands (I: ν(CCl₄) 1694 cm⁻¹; II: ν(CCl₄) 1680 cm⁻¹) and similar mass spectra (M⁺, m/e 283) with only minor differences in peak intensities. Their 100 Mc./sec. ¹H NMR spectra show a sharp three-proton singlet assigned to an aryl C-methyl group (δ 2.60 in I, δ 2.63 in II) and similar ABX systems (670-740 c./sec.) for three aromatic protons. NMR analysis (including double irradiation) demonstrates isoelaeocarpine is the C-7 epimer of elaeocarpine: the C-7 proton of elaeocarpine appears as a broad multiplet at δ 4.16 with coupling constants J₇,₈ 11.8 c./sec. and +(J₇,₆β + J₇,₆α) 7.8 c./sec. (consistent with trans-diaxial couplings), while the C-7 proton of isoelaeocarpine is a narrow multiplet at δ 4.64 with small coupling constants (consistent with C-7, C-8 cis-stereochemistry). The C-8 proton signals (quartets at δ 2.61 in I, δ 2.42 in II) confirm identical C-8, C-9 stereochemistry in both alkaloids. Proton assignments in the NMR spectra were confirmed by examining C-8 deuterio-substituted derivatives of I and II in CD₃OD containing a trace of NaOD.

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