“…After 5 min, the mixture was poured into water (25 mL) and extracted with ether, the combined organic extracts dried (K2C03), and the solvent removed in vacuo. The acid-sensitive enone 28 thus obtained (65.5 mg, 92%) was used without further purification: IR (neat) 3600-3200 (m), 1710 (s), 1680 (s) cm"1; NMR (250 MHz, CDC13) b 7.34-7.29 (m, 5 ), 4.71 (t, J = 5 Hz, 1 H), 4.44 (center of AB, J = 11.7 Hz, 2 ), 4.02 (d, J = 8 Hz, 1 H), 3.57 (br s, 1 ), 2.8-0.8 (m, 11 ), 1.26 (s, 3 ), 1.11 (s, 3 ), 1.04 (s, 3 H). Enone 28 (200 mg, 0.5 mmol) was dissolved in a mixture of 16 mL of dry pyridine and 125 mL of dry CH2C12 under nitrogen. The mixture was cooled to 0 °C and thionyl chloride (1.5 mL, 20.5 mmol) added dropwise.…”