反应详情

温度

90 °C

To a solution methyl 3-[1-(6-chloropyridazin-3-yl)-2-oxo-4-(trimethylsilyl)but-3-yn-1-yl]-4methoxybenzoate (5.58 g, 13.4 mmol) in THF (200 mL) was added TBAF (20.0 mL, 20 mmol) at 0° C. After 10 min the reaction was complete by TLC analysis and diluted with H2O/EtOAc (1/1). The organic layer was washed with H2O, brine, dried over MgSO4 and concentrated to yield an oil. The crude material was dissolved in NMP (25 mL) and heated to 90° C. for 0.5 hr. The completed reaction was poured into 500 mL of ice water and the solid precipitate was collected and dried.

1. washThe organic layer was washed with H2O, brine
2. dry with materialdried over MgSO4
3. concentrationconcentrated
4. customto yield an oil
5. customThe completed reaction
6. customthe solid precipitate was collected
7. customdried