“…The residue was purified by radial chromatography (2% MeOHCH2Cl2, EtOAc-Hex, 1:1) to give 78 mg (78%) of enone 8 as a white powder: mp 215-219°C, [R] 23 D -2.9°(c 1.0, CH2Cl2); IR (KBr) νmax 3570,2972,1753,1740,1716,1664,1599,1451,1372,1242,1087,1070,1024,959,824,807,720,668 (1H, br s), 5.50 (1H, br s), 6.25 (1H, d, J ) 10.7 Hz), 6.88 (1H, d, J ) 10.7 Hz), 7.43 (2H, t, J ) 7.5 Hz, Hm-Ph), 7.58 (1H, t, J ) 7.5 Hz, Hp-Ph), 7.91 (2H, br d, J ) 7.5 Hz, Ho-Ph, in a 4:1 ratio with δ 8.03), 8.03 (2H, br d, J ) 7.5 Hz, Ho-Ph); 13 C NMR (CDCl3, 75 MHz) δ 8. 8,12.5,14.0,26.6 (4 CH3,20.7,21.1,21.2 [3 CH3,], 27.5, 33.6 (2 CH2, C-2 + C-6), 39.0 (CH, C-3), 45.1 (C,49.6 (CH2,, 59.0 (C, C-1), 69. 5,70.1,74.0,77.2 (4 CH,75.2 (C,114.3 (CH2,, 128.8, 129.5 (2 CH, C-2′ + C-3′), 129.4 (C, C-1′), 133.5 (CH, C-4′), 145.0, 147.0 (2 C, C-4 + C-12), 163.6 (C, O2CPh), 163.9 (C,169.5,169.8,169.9 [3 C, (b) From NMO-TPAP Oxidation.…”