反应详情

To a solution of 31 (˜17 mmol) in t-butylacetate (70 mL) was added perchloric acid (1.23 mL, 20.4 mmol). After 3 h, water was added (50 mL). The layers were separated. The organic layer was washed with a saturated solution of NaHCO3. The organic layer was dried, filtered, and concentrated in vacuo. The crude material was purified by column chromatography (EtOAc/hexanes) to give 7.22 g of 32 and 1.58 g of 31. 1H-NMR: 400 MHz, (CD3OH) δ: 7.82 (s, 1H), 5.59 (s, 1H), 4.08-4.25 (m, 2H), 2.55 (s, 3H), 1.20 (s, 9H), 1.16 (t, 3H, J=7 Hz). LCMS-ESI+: calc'd for C17H20BrF3NO6S2: 534.0 (M+H+); Found: 534.1 (M+H+).

1. customThe layers were separated
2. washThe organic layer was washed with a saturated solution of NaHCO3
3. customThe organic layer was dried
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe crude material was purified by column chromatography (EtOAc/hexanes)