“…The remaining solid was dissolved in hexane and first frozen in liquid N 2 and then stored at Ϫ25 ЊC for several days to afford 9 as a beige solid (1.85 g, 49%) (it was too labile for elemental analysis), mp 45-50 ЊC (decomp.). 1 H NMR: δ 0.89 (s, 9H, Bu t ), 3.05 (vbr quartet, 4H, CH 2 ), 6.49-6.54 (m, 4H, Ph); 1 H NMR (343 K): δ 0.92 (s, 9H, Bu t ), 2.99, 3.02, 3.12, 3.15 (AB-type, 4H, CH 2 ), 6.54-6.59 (m, 4H, Ph); 13 C NMR (343 K): δ 29.83 (CMe 3 ), 34.17 (CMe 3 ), 59.52 (CH 2 ), 117.8, 120.75, 140.93 (Ph); 27 Al NMR: δ 115.2 ∆w ½ 3 kHz. MS (m/z, %): 273 (6%, [M Ϫ Cl] ϩ ).…”