[CH2:1]([PH:5](=[O:10])[CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4].C([Mg]Br)CCC.C(OP([O-])OCC)C.[CH3:25][Si:26](Cl)([CH3:28])[CH3:27]>C1(C)C=CC=CC=1.C(N(CC)CC)C>[CH2:1]([P:5]([CH2:6][CH2:7][CH2:8][CH3:9])[O:10][Si:26]([CH3:28])([CH3:27])[CH3:25])[CH2:2][CH2:3][CH3:4]
The procedure described in Tetrahedron, 1967, 23, 1065 (M. Grayson et al.) was followed. Dibutylphosphine oxide, prepared from butyl magnesium bromide and diethylphosphite, (3.3 g, 20 mmol) and triethylamine (2.02 l g, 20 mml) were dissolved in toluene (20 mL) and treated with a solution of trimethylsilyl chloride (2.17 g, 20 mmol) in toluene (5 mL) at room temperature. The solution got very warm and a precipitate formed immediately. The mixture was heated at 80° C. for two hours, then filtered, washed with toluene, and concentrated. Kugelrohr distillation a 80° C. (1.5 mmHg) afforded 4.1 g (86%) of the desired product. 1H NMR (CDCl3) δ1.8-1.2 (m, 6H), 1.1-0.7 (m, 3H), 0.17 (s, 9H).
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