ScienceDirect - Tetrahedron Letters : Application of long range 1H/13C heteronuclear correlation spectroscopy (LR HETCOSY) to structure elucidation: The structure of murayaquinone

Tetrahedron Letters
Volume 27, Issue 2, 1986, Pages 143-146

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doi:10.1016/S0040-4039(00)83962-3

Application of long range ¹H/¹³C heteronuclear correlation spectroscopy (LR HETCOSY) to structure elucidation: The structure of murayaquinone

Yukiharu Sato^a, Rodger Kohnert and Steven J. Gould, ^*

Department of Chemistry, Oregon State University Corvallis, Oregon 97331 U.S.A.

^a On leave from Tamagawa University, 6-1-1 Tamagawa Gakuen, Machida-shi, Tokyo 194, Japan

Received 21 May 1985.

Available online 8 March 2001.

Abstract

The structure of a polyketide-derived, -phenanthraquinone streptomyces metabolite has been deduced from interpretation of a 2D heteronuclear correlation experiment that reveals long range ¹H-¹³C couplings.

References

S. Ito, T. Matsuya, S. Ømura, H. Otani, A. Nakagawa, H. Takeshima, Y. Iwai and T. Hata J. Antibiot. 23 (1970), p. 315. View Record in Scopus | Cited By in Scopus (23)
T Hata, S. Omura, Y. Iwai, A. Nakagawa, M. Otani, S. Ito and T. Matsuya J. Antibiot. 24 (1971), p. 353. View Record in Scopus | Cited By in Scopus (21)

S. Ømura, A. Nakagawa, H. Yamada, T. Hata, A. Furusaki and T. Watanabe Chem. Pharm. Bull. 19 (1971), p. 2428.
S. Ømura, A. Nakagawa, H. Yamada, T. Hata, A. Furusaki and T. Watanabe Chem. Pharm. Bull. 21 (1973), p. 931. View Record in Scopus | Cited By in Scopus (31)

Y. Sato and S.J. Gould Tetrahedron Lett. 26 (1985), p. 4023. Abstract | PDF (200 K) | View Record in Scopus | Cited By in Scopus (5)

The pulse pulse sequence provides both one-bond and long range heteronuclear couplings, and is described in H. Bleich, S. Gould, P. Pitner and J. Wilde J. Mag. Reson. 56 (1984), p. 515. Article | PDF (162 K) | View Record in Scopus | Cited By in Scopus (3)
For an example of its use for ¹H/¹³C couplings see Y. Sato, M. Geckle and S.J. Gould Tetrahedron Lett. 26 (1985), p. 4019. Abstract | PDF (222 K) | View Record in Scopus | Cited By in Scopus (5)

Recently, other approaches for detecting long range J_CHs have been published H. Seto, K. Furihata, N. Otake, Y. Itoh, S. Takahashi, Tl Haneishi and M. Ohuchi Tetrahedron Lett. 25 (1984), p. 337. Abstract | PDF (287 K) | View Record in Scopus | Cited By in Scopus (3)
H. Kessler, C. Griesinger and J. Lautz Angew. Chem. 23 (1984), p. 444 Int. Ed. Engl. . Full Text via CrossRef
W.F. Reynolds, R.G. Enriquez, L.I. Escobar and X. Lozoya Can. J. Chem. 62 (1984), p. 2421. Full Text via CrossRef
J.P. Kintzinger, P. Maltese, M. Bourdonneau and C. Brevard Tetrahedron Lett. 25 (1984), p. 6007. Abstract | PDF (219 K) | View Record in Scopus | Cited By in Scopus (0)

UVmax (MeOH) 524 ( var epsilon =4485), 401 (=3175), 288 (=13920), 242 nm (=18284); ¹H NMR (CDCl₃, 400.13 MHz) δ1.00 (3H, t, J = 7.5 Hz), 1.71 (2H, m), 2.20 (3H, s), 2.78 (2H, t, J = 7.5 Hz), 6.94 (1H, d, J = 8.6 Hz), 7.31 (1H, s), 7.40 (1H, d, J = 8.3 Hz), 7.54 (1H, dd, J = 8.6 and 8,3 Hz), 12.27 (1H,s), 12.72 (1H, s); ¹³C NMR (CDCl₃, 100.6 MHz) δ205.4 (s), 182.6 (s), 182.2 (s), 166.1 (s), 165.0 (s), 150.0 s), 139.4 (d), 135.0 (s), 132.8 (s), 126.2 (s), 119.6 (d), 115.9 (d), 115.3 (s), 114.8 (s), 113.1 (d), 44.9 (t), 17.3 (t), 13.8 (q), 12.0 (q); HRMS (70 ev) m/z calcd. for C₁₉H₁₆O₅: 324.0097, fnd. 324.1006.

J. Polonsky, B.C. Johnson, P. Cohen and E. Lederer Bull. Soc. Chim. Fr. (1963), p. 1909.

M. Lounasmaa and J. Zylber Bull. Soc. Chim. Fr. (1969), p. 3100. View Record in Scopus | Cited By in Scopus (3)

B. Krone, A. Hinrichs and A. Zeeck J. Antibiot. 34 (1981), p. 1538. View Record in Scopus | Cited By in Scopus (1)

Tetrahedron Letters
Volume 27, Issue 2, 1986, Pages 143-146

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