反应详情

To a solution of Compound 3 in Et2O (120 ml) were added acetylsalicyloyl chloride (Compound 4) (5.9 g, 0.028 mol) and triethylamine (Et3N) (6.6 ml, 0.047 mol) in sequence at RT. The reaction mixture was stirred at RT under argon for 3 days. The reaction mixture was diluted with EtOAc (100 ml) and washed with aqueous saturated NaHCO3 (3×100 ml), brine (1×100 ml), and dried over anhydrous Na2SO4. The crude product obtained upon concentration was purified by column chromatography (elution solvent: 5% EtOAc in hexanes) to produce 9.4 g of Compound 5 in 100% yield.

1. washwashed with aqueous saturated NaHCO3 (3×100 ml), brine (1×100 ml)
2. dry with materialdried over anhydrous Na2SO4
3. customThe crude product obtained upon concentration
4. customwas purified by column chromatography (elution solvent: 5% EtOAc in hexanes)