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Stage #1: With n-butyllithium In tetrahydrofuran; hexane at -78℃; for 1.33333 h; Stage #2: With 1,2-dibromo-1,1,2,2-tetrachloroethane In tetrahydrofuran; hexane at -78 - 20℃;
A solution of 209-2 (50.0 g, 183.8 mmol) in dry THF cooled to -78° C. and n-BuLi (81 ml, 2.5 M in hexane) was added over 20 minutes. The resulted solution was maintained at -78° C. for 1 h, and then a solution of BrCl2CCCl2Br (71.0 g, 220.5 mmol) in dry THF was added. The mixture was stirred -78° C. for 30 min and allowed to warm slowly to room temperature. The solvent was removed under vacuum and the residue was partitioned between EtOAc and water. The organic layer was dried over anhydrous Na2SO4 and concentrated. The crude product was purified by column chromatography (5percent ethyl acetate in petroleum ether to 20percent ethyl acetate in petroleum ether as the eluent) to afford 209-3 (37 g, 58percent yield). MS-ESI: m/z=351.0 [M+1]+
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