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3. Extractive workup with ether and chromatographic purification of the crude product on silica gel gave the bis-TMS-silylated aldol adducts in 96% yield as a mixture of diastereomers.
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11
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0037539964
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note
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+, 38), 206 (50), 151 (100).
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12
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0038215432
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note
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3) δ 0.06 (s, 3H), 0.09 (s, 3H), 0.89 (s, 9H), 4.61 (m, 1H), 5.00 (m, 1H), 6,19 (dd, 1H, J = 5.8, 1.8 Hz), 6.22 (dd, 1H, J = 16, 5.6 Hz), 6.71 (d, 1H, J = 16 Hz), 7.15-7.45 (m, 5H), 7.49 (dd, 1H, J = 5.8, 1.6 Hz); EIMS m/z 315 (M-15).
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13
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0000687154
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Cf: (a) G. Casiraghi, L. Colombo, G. Rassu, P. Spanu, G. G. Fava, M. F. Belicchi, Tetrahedron, 1990, 46, 5807. (b) G. Rassu, L. Pinna, P. Spanu, F. Zanardi, L. Battistini, G. Casiraghi, J. Org. Chem., 1997, 62, 4513. (c) M. Szlosek, X. Franck, B. Figadere, A. Cave, J. Org. Chem., 1998, 63, 5169.
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