Following reported procedure, 12 trimethylsilyl triflate (400 μL, 2.20 mmol, 1.10 equiv) was added to a suspension of BIOH-b (25) (648 mg, 2.00 mmol, 1.00 equiv) in CH2Cl2 (10 mL) at RT. The resulting yellow mixture was stirred for 1 h, followed by the dropwise addition of trimethyl(phenylethynyl)silane (430 μL, 2.20 mmol, 1.10 equiv). The resulting suspension was stirred for 6 h at RT, during this time a yellow suspension was formed. A saturated solution of NaHCO3 (10 mL) was then added. The two layers were separated and the aqueous layer was extracted with DCM (10 mL). The combined organic extracts were dried over MgSO4, filtered and evaporated under reduced pressure. The resulting solid was recrystallized in CH3CN ( mL) and a few EtOH to afford 2h (306 mg, 0.752 mmol, 38%) as a colorless solid. Consistent with reported data. 12