5432
M. Essers et al. / Tetrahedron Letters 42 (2001) 5429–5433
Tetrahedron 2000, 56, 3539–3545; (f) Essers, M.; Haufe,
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2H), 4.92 (dd, J=3.6, 2.4 Hz, 2H), 10.38 (br s, 2H). 13C
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(dt, J=10.8 Hz), 93.5 (dd, J=222.0 Hz, 18.5 Hz), 167.5
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333K): l 72.1 (1O), 259.9 (4O). GC/MS (of the TMS-
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(20), 221 (26), 187 (10), 185 147 (26), 77 (42), 73 (100), 45
(9). Anal. calcd for C8H8F2O5: C, 43.25, H, 3.63; found:
C, 43.36; H, 3.86.
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Copies of the data can be obtained, free of charge, on
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1
27. Compound 5: H NMR (300 MHz, CD3OCD3): l 1.75–
2.01 (m, 3H), 2.07–2.21 (m, 1H), 3.58 (d, J=13.1 Hz,
1H), 4.92–4.96 (m, 1H), 4.97–5.01 (m, 1H). 13C NMR (75
MHz, CD3OCD3): l 22.7 (dt, J=5.1 Hz), 27.3 (t), 54.0
(d, J=21.6 Hz), 82.6 (dd, J=3.8 Hz), 80.4 (dd, J=24.2
Hz), 98.5 (d, J=216.2 Hz), 168.9 (d, J=26.7 Hz), 168.6
(d, J=7.6 Hz). 19F NMR (282 MHz, CD3OCD3): l
−183.0 (d, J=13.1 Hz). 17O NMR (49 MHz, CH3CN,
333K): l 79.2 (1O), 302.2 (1O), 377.0 (2O). GC/MS m/e