反应详情

Add trifluoroacetic acid (5 mL) to a solution of (2-chloro-phenyl)-[3-(2-trimethylsilanyl-ethoxymethoxy)-pyridin-2-yl]-methanone (195 mg, 0.54 mmol) in CH2Cl2 (3 mL), stir for 30 minutes. Concentrate; dissolve in 20% i-PrOH/CHCl3, wash with saturated NaHCO3 solution (×2). Dry the combined organic layers over MgSO4 and concentrate. Purify the residue by flash chromatography on silica gel eluting with 0-30% Et2O/hexanes to afford the title compound (102 mg, 82%) as white solid. MS(IS) 233.9 (M+1). TLC: Rf=0.20 (25% Et2O/hexanes).

1. concentrationConcentrate
2. dissolutiondissolve in 20% i-PrOH/CHCl3
3. washwash with saturated NaHCO3 solution (×2)
4. dry with materialDry the combined organic layers over MgSO4
5. concentrationconcentrate
6. customPurify the residue by flash chromatography on silica gel eluting with 0-30% Et2O/hexanes