Strukturermittlung und Synthese des Disaccharidfragments B-A von Mithramycin†
First published: Januar 1983
No abstract is available for this article.
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- 4
(a)
Fp = 157°C, [α]20D 175 (Essigester); 1H-NMR (C6D6, 400 MHz): 1-H δ = 4.57 dd, 1′-H 5.19 dd; J(1,2a) = 3.5, J(1,2e) = 1.0, J(1′,2a') = 3.3, J(1′,2e') = 1.2 Hz; b) 72%, Fp = 140°C, [α]20D 200 (Aceton); c) Sirup, [α]20D 19 (Essigester); 1H-NMR (CDCl3, 400 MHz): 1-H δ = 4.84 dd, 3-H 4.16 ddd, 4-H 5.21 dd, 1′-H 4.62 dd; J(1,2a) = 3.4, J(1,2e) = 1.2, J(2a,3) = 12.0, J(2e,3) = 5.1, J(3,4) = 3.1, J(4,5) = 1.0, J(1′,2a') = 9.7, J(1′,2e') = 2.0 Hz; d) Sirup, [α]20D 38 (Aceton); 1H-NMR ([D6]Aceton, 270 MHz): 1-H δ = 4.70 dd, 1′-H 4.72 dd; J(1,2a) = 3.5, J(1,2e) = 1.2, J(1′,2a') = 9.7, J(1′,2e') = 2.0 Hz; e) Fp = 145°C, [α]20D 169 (Essigester); 1H-NMR (CDCl3, 400 MHz): 1-H δ = 4.82 dd, 1′-H 4.95 dd; J(1,2a) = 3.2, J(1,2e) = 1.1, J(1′,2a') = 3.3, J(1′,2e') = 1.1 Hz; f) Fp = 134°C, [α]20D 64 (Aceton); g) Fp = 92°C, [α]20D 72 (Essigester); 1H-NMR (CDCl3, 400 MHz): 1-H δ = 4.84 dd, 3-H 5.18 ddd, 4-H 3.87 dd, 1′-H 4.55 dd; J(1,2a) = 3.2, J(1,2e) = 1.1, J(2a,3) = 12.2, J(2e,3) = 5.0, J(3,4) = 2.8, J(4,5) = 1.2, J(1′,2e') = 9.7, J(1′,2e') = 2.0 Hz; h) Sirup, [α]20D 37 (Aceton); 1H-NMR ([D6]Aceton, 270 MHz): 1-H δ = 4.67 dd, 1′-H 4.82 dd; J(1,2a) = 3.4, J(1′,2a') = 9.7, J(1′,2e') = 2.0 Hz; i) 1H-NMR (CDCl3, 400 MHz): 3A-H δ = 3.92 ddd, 4A-H 5.13 dd; J(2aA,3A) = 12.1, J(2eA,3A) = 4.6, J(3A,4A) = 3.2, J(4A,5A) = 0.9 Hz.
- 5
Für Mithramycin danken wir
Dr. H. Krisch,
Pfizer GmbH, Karlsruhe.
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