“…The extract was combined with the organic phase and dried over anhydrous MgS04. Evaporation of the solvent at reduced pressure gave 1.09 g of crude 4. Crystallization of 4 from CHClg/acetone gave 761 mg (87% yield) of 4 as an off-white solid: mp 270-271 °C; 18C NMR 61.9 (C-3, C-3', C-5, and C-5'), 58.5 (C-4 and C-4'), 46.5 (C-6, C-6', C-10, and C-100, 46.1 (C-l and C-l'), 45.8 (C-2, C-2', C-9, and C-9'), 34.3 (C-7 and C-7'), 32.3 (C-8 and C-8'); NMR 2.80 (AB multiplet, 4 H), 2.33 (m, 1H), 2.22 (m, 4 ), 2.14 (bs, 4 ), 1.59 (bd, J = 2.9 Hz, 2 H); HRMS caled for CgoHggBrg (M+ -Br) 502.9579, found 502.9547.…”