反应详情

To a solution of 1-phenyl-4-(tetrahydro-2H-pyran-2-yloxy)but-2-yn-1-ol (3.0 g, 12.2 mmol) in DCM (50 mL) was added DMP (10.0 g, 24.4 mmol). The resulting solution was stirred for 30 min at room temperature and then the reaction mixture was poured into NaHCO3/NaS2O3 solution and stirred for overnight, extracted with DCM (3×150 mL), dried over anhydrous sodium sulfate and then concentrated in vacuo to give a residue. The residue was purified by silica gel column chromatography (3% ethyl acetate in petroleum ether) to afford 1-phenyl-4-(tetrahydro-2H-pyran-2-yloxy)but-2-yn-1-one as a light yellow oil (2.4 g).

1. stirringstirred for overnight
2. extractionextracted with DCM (3×150 mL)
3. dry with materialdried over anhydrous sodium sulfate
4. concentrationconcentrated in vacuo
5. customto give a residue
6. customThe residue was purified by silica gel column chromatography (3% ethyl acetate in petroleum ether)