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- Preparation of complex 3: To a solution of 0.5 g (1 mmol) complex 1 in diethyl ether (20 mL), LiAlH4 (1 mL of 1 M solution in diethyl ether) at was added –25°C over 5 min. The resulting yellow solution is stirred for 2 h and allowed to warm up to r.t. After this, it was cooled to 0°C and quenched with water. The reaction mixture was extracted with diethyl ether (3 × 15 mL). Solvents were removed at reduced pressure, and the residue was chromatographed on silica gel with pentane as the eluent. Yield 38%, 0.2 g. Colorless solid. 31P (CDCl3): 180.7 (J 1 P-W = 316 Hz, J 3 P-H = 21 Hz); 1H (CDCl3): 1.41 (18H, d, J 3 P-H = 21 Hz); 13C (CDCl3): 197.9 (C≡O, d, J 2 C-P = 40 Hz, J 1 C-W = 141 Hz), 195.3 (C≡O, d, J 2 C-P = 7.7Hz, J 1 C-W = 128Hz), 30.0 (C-P, d, J 1 C-P = 5.4 Hz), 24.1 (CH3, d, J 2 C-P = 10 Hz). IR (CH2Cl2) ν co = 2084, 1974, 1958 cm-1 .
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