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Ligands Preparation (Scheme 1) The Preparation of Ligand 3 A 10 mL Schlenk flask was charged with diol 2 (100 mg, 0.78 mmol, DMAP (20 mg, Et3N (160 mg, 1.6 mmol) and THF (5 mL) under nitrogen. The mixture was stirred at 0°C. A solution of chlorodiphenylphosphine (0.3 mL, 1.56 mmol) in THF (2 mL) was added dropwise with stirring, then stirred at r.t. for 24 h. After filtration, the solvent was removed under vacuum. The crude product was purified through flash chromatography to give pure product as a thick liquid; yield 233 mg (47, MS (EI, m/z, 496 [M, 1H NMR (400 MHz, CDCl3, δ =7.44-7.13 (m, 20 H, Ph, 4.70-4.69 (b, 2 H, C2 and C5, 2.25 (s, 2 H, bridgehead, 1.92 (d, 2 H, endo of C3 and C5, 1.69 (m, 2 H, exo of C3 and C5, 1.23 (s, 2 H, bridge, 13C NMR (100 MHz, CDCl3, δ, 149.678-122.009 (Ph, 75.628 (O-C, 42.500(bridgehead, 34.849 (bridge, 28.965 C3 and
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2 [M + K]: 795.1462; found: 795.1461.
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