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Ϫ Major Me 4 Si ( 1 H) and CDCl 3 ( 13 C, δ ϭ 77.05). Standard correlation techanomer: 1 H NMR (400 MHz, CDCl 3 ): δ ϭ 3.81Ϫ3.92 (m, 4 H, 5 aniques were used for assignments. Ϫ Mass spectra: Varian CH 7 H, 5 b -H, SCH 2 Ph), 3.95Ϫ3.97 (m, 1 H, 4-H), 3.99 (dd, 1 H, 2-H), (EI) and VG Analytical 70-250 S (FAB, HRMS). Ϫ TLC was car-4.31Ϫ4.63 (m, 7 H, 3-H, OCH 2 Ph), 4.98 (d, 1 H, 1-H), 7.18Ϫ7.37 ried out on Merck PF 254 foils (detection: UV light, iodine vapour, (m, 20 H, ArH); J 1,2 ϭ 2.2, J 2,3 ϭ 4.7 Hz. Ϫ 13 C NMR (101 MHz, or EtOH/H 2 SO 4 spray/200°C), and column chromatography on CDCl 3 ): δ ϭ 35.55 (SCH 2 Ph), 68.75 (C-5), 71.79, 71.89, 73.46 Merck Kieselgel 60 (70Ϫ230 mesh). Solvents were purified and (OCH 2 Ph), 81.02 (C-3), 82.01 (C-2), 86.38 (C-1), 87.04 (C-4), for dried according to standard laboratory procedures. [23] signals of aromatic C atoms see note below. Ϫ Minor anomer: 1 H NMR (400 MHz, CDCl 3 ): δ ϭ 3.70 (dd, 1 H, 5 a -H), 3.79 (dd, 1 Methyl 2,3,5-Tri-O-benzyl--xylo-furanoside (3): Compound 3 was H, 5 b -H), 3.81Ϫ3.92 (m, 2 H, SCH 2 Ph), 4.08Ϫ4.11 (m, 2 H, 2-H, prepared from methyl -xylo-furanoside (2) according to standard 4-H), 4.31Ϫ4.63 (m, 7 H, 3-H, OCH 2 Ph), 5.44 (d, 1 H, 1-H), procedures. [5,16] Compound 3 has been mentioned by Yoshimura et 7.18Ϫ7.37 (m, 20 H, ArH); J 1,2 ϭ 5.0, J 4,5a ϭ 6.2, J 4,5b ϭ 5.5, al. [11] without data which are therefore dealt with here. Ϫ IR (film):
J 5a,5b ϭ 10.3 Hz. Ϫ 13 C NMR (101 MHz, CDCl 3 ): δ ϭ 34.29
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