反应详情

温度

110 °C

To a solution of 1-[5-(2,2-dimethyl-1,3-dioxolan-4-yl)pyridin-2-yl]-5-[4-(methylsulfonyl)phenyl]-6-(tetrahydro-2H-pyran-4-yl)hexane-1,4-dione (232 mg) in acetic acid (5 mL) was added ammonium acetate (540 mg), 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 to give a crude product (218 mg). To a solution of the obtained crude product in tetrahydrofuran (5 mL) was added 1M hydrochloric acid (5 mL), and the mixture was stirred at 50° C. for 4 hr. The reaction mixture was diluted with ethyl acetate and washed with saturated aqueous sodium hydrogen carbonate. The ethyl acetate layer was washed with saturated brine, dried (MgSO4) and concentrated. The residue was subjected to preparative HPLC to give the title compound (155 mg, yield 78%) as a colorless amorphous solid. MS: 471 (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
6. customto give a crude product (218 mg)
7. stirringthe mixture was stirred at 50° C. for 4 hr
8. washwashed with saturated aqueous sodium hydrogen carbonate
9. washThe ethyl acetate layer was washed with saturated brine
10. dry with materialdried (MgSO4)
11. concentrationconcentrated