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35548956245
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31P NMR at δ = 23.9 (unassigned).
-
31P NMR at δ = 23.9 (unassigned).
-
-
-
-
53
-
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35548975024
-
-
Compound 15 was more difficult to obtain in a pure form, probably because of conversion into 16.
-
Compound 15 was more difficult to obtain in a pure form, probably because of conversion into 16.
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54
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35549011739
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When we tried to separate this compound from 5,5-diethyl-2-(3-methylbuta- 1,2-dienyl)-1,3,2-dioxaphosphinane 2-oxide using column chromatography, a small quantity of an additional species [δ(P) -12.2] was noticed in a few fractions.
-
When we tried to separate this compound from 5,5-diethyl-2-(3-methylbuta- 1,2-dienyl)-1,3,2-dioxaphosphinane 2-oxide using column chromatography, a small quantity of an additional species [δ(P) -12.2] was noticed in a few fractions.
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55
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84985610223
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33645462025
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and references cited therein. Such trienes are perhaps useful in cyclization reactions, see
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Such trienes are perhaps useful in cyclization reactions, see: Murahashi, T.; Nakashima, H.; Nagai, T.; Mino, Y.; Okuno, T.; Jalil, M. A.; Kurosawa, H. J. Am. Chem. Soc. 2006, 128, 4377; and references cited therein.
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Organic Chemistry of Sulfur; Oae, S., Ed.; Plenum: New York, 1977.
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(a) Organic Chemistry of Sulfur; Oae, S., Ed.; Plenum: New York, 1977.
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60
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35548939713
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IR (KBr, 3399, 2928, 1570, 1335, 1206, 1057, 1005 cm-1; 1H NMR (400 MHz, CDCl3, δ, 0.99 and 1.10 (2 s, 6 H, 2 CH3, 2.01-2.06 [2 m due to coupling to phosphorus and CH2 with J <5.0 Hz, 6 H, C(CH3) 2, 3.34 (dd, J ∼4.0 Hz, J ∼20.6 Hz, 2 H, PCH2, 3.79-4.95 (m, 9 H, CH2OH, CHCH2OH, 2 CHOH, OCH2, 5.90 (d, J ∼7.0 Hz, OCHN of ribose, 8.13 (s, 1 H, nucleobase-H, 8.62 s, 1 H, Nucleobase-H, LC-MS showed a peak at m/z 503
-
2), 5.90 (d, J ∼7.0 Hz, OCHN of ribose), 8.13 (s, 1 H, nucleobase-H) , 8.62 (s, 1 H, Nucleobase-H); LC-MS showed a peak at m/z 503.
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(b) Sheldrick, G. M. SHELXTL NT Crystal Structure Analysis Package, version 5.10; Bruker AXS, Analytical X-ray System: WI USA, 1999.
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