*3.3. Large-Scale Experiment*

A solution of (*R*,*R*)-PhBOX (200 mg, 0.60 mmol) and CuCN (53.7 mg, 0.60 mmol) in CH2Cl2 (24 mL) was stirred for 3 h at 40 ◦C. The reaction mixture was allowed to cool to room temperature and filtered into a round bottom flask using a cotton plug. After removal of the solvent under reduced pressure, the resulting solid was dried in vacuo for 1 h. To the round-bottom flask containing CuCN/(*R*,*R*)-PhBOX was added a solution of glycerol (553 mg, 6.0 mmol) in acetone (24 mL), and the resulting mixture was stirred for 10 min at room temperature. To the mixture was successively added Na2CO3 (950 mg, 9.0 mmol) and TsCl (1.37 g, 7.2 mmol), and the mixture was stirred for 9 h at room temperature. The reaction was quenched with saturated aqueous NH4Cl, and the resulting mixture was extracted with AcOEt. Combined organic layers were washed with brine, dried over Na2SO4, filtered, and concentrated under reduced pressure. The crude product was purified by silica gel column chromatography (hexane/AcOEt = 1/2) to afford (*R*)-**2** (1.30 g, 5.28 mmol, 88% yield, 93% ee).
