反应详情

温度

110 °C

To a solution of 5-[4-(cyclopropylsulfonyl)phenyl]-1-[5-(1,3-dioxolan-2-yl)pyridin-2-yl]-6-(tetrahydro-2H-pyran-4-yl)hexane-1,4-dione (4.40 g) in acetic acid (35 mL) was added ammonium acetate (10.3 g), and the mixture was stirred at 110° C. for 45 min. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate and washed with water. The ethyl acetate layer was washed with saturated aqueous sodium hydrogen carbonate and saturated brine, dried (MgSO4) and concentrated. The residue was subjected to silica gel column chromatography, and the title compound (3.22 g, yield 83%) was obtained as a yellow amorphous solid from a fraction eluted with ethyl acetate-hexane (2:1, volume ratio). MS: 465 (MH+).

1. temperatureAfter cooling to room temperature
2. washwashed with water
3. washThe ethyl acetate layer was washed with saturated aqueous sodium hydrogen carbonate and saturated brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated