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To a stirred solution of phosphoramidite ligand (R,S,S)-141 (1.95 g, 3.61 mmol) in Et2O (140 mL) was added CuTC (346 mg, 1.81 mmol) at 22 °C. The mixture so obtained was stirred at that temperature for 30 min and then cooled to ?30 °C before Me3Al (54.0 mL, 2.0 M in hexane, 108 mmol) and a solution of 2-methylcyclohexenone 112 (10.0 g, 90.8 mmol) in Et2O (20 mL) were sequentially added. The reaction mixture was stirred at ?30 °C for 2.5 h before THF (140 mL), HMPA (40.7 g, 39.5 mL, 227 mmol), and MeLi (56.5 mL, 1.6 M in Et2O, 90.8 mmol) were sequentially added. The reaction mixture was stirred at ?30 °C for 20 min before a solution of allyl iodide 123 (30.0 g, 118 mmol) in THF (20 mL) was added. The resultant mixture was stirred at ?30 °C for 24 h, then warmed to ?10 °C and stirred at that temperature for 24 h, and then warmed to 0 °C and stirred at that temperature for 48 h before it was diluted with Et2O (500 mL) and quenched with saturated aq. NH4Cl (300 mL). The mixture so obtained was filtered through a short plug of Celite. The organic layer was separated, and the aqueous layer was extracted with Et2O (3 × 500 mL). The combined organic phases were washed with brine (2 × 100 mL), dried over anhydrous Na2SO4, and filtered. The solvent was evaporated under vacuum, and the residue was subjected to flash column chromatography for purification using Et2O/petroleum ether (1:50 → 1:30) as eluent to give cyclohexanone 15 (14.9 g, 65%, 3.8:1 dr) as a pale yellow oil. 发自小木虫Android客户端 |
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