反应详情

To a solution of diisopropylamine (5.6 mL, 40 mmol) in dry THF (60 mL) at -10° C. was added 1.6M BuLi (25 mL, 40 mmol). After 30 min, a solution of 2-iodophenylacetic acid (5.24 g, 20 mmol) in THF (20 mL) was slowly added. The solution was stirred for 1 h, at which point iodoethane (1.6 mL, 117 mmol) was added. After 2 h at r.t. the reaction was quenched with 0.5M NH4OAc solution and 6M HCl (10mL) and the product was extracted with EtOAc. The organic layer was dried (MgSO4) and evaporated to give an oily residue which was purified by flash chromatography (15:85 EtOAc:hexane containing 5% AcOH) to give 4.37 g of the title compound as an off-white solid.

1. additionwas added
2. customAfter 2 h at r.t. the reaction was quenched with 0.5M NH4OAc solution and 6M HCl (10mL)
3. extractionthe product was extracted with EtOAc
4. dry with materialThe organic layer was dried (MgSO4)
5. customevaporated
6. customto give an oily residue which
7. customwas purified by flash chromatography (15:85 EtOAc:hexane containing 5% AcOH)