反应详情

To a solution of the aldehyde from Example 3 (160 mg) and 2-methyl-2-butene (6 mL) in 2-methyl-2-propanol (35 mL) was added a solution of NaClO2 (1 g) and NaH2PO4 (1 g) in 10 mL of H2O. The mixture was stirred for 2 h at r.t., and concentrated. The residue was then taken into 50 mL of pH 7 buffer solution (1M) and extracted with EtOAc (50 mL). The extract was dried over MgSO4 and concentrated. The residue was purified by flash chromatography, eluting with 3:1 EtOAc/hexane containing 1% HOAc to give 150 mg of the title compound as a white solid.

1. concentrationconcentrated
2. extractionextracted with EtOAc (50 mL)
3. dry with materialThe extract was dried over MgSO4
4. concentrationconcentrated
5. customThe residue was purified by flash chromatography
6. washeluting with 3:1 EtOAc/hexane containing 1% HOAc