反应详情

温度

85 °C

To 2-(2,2-difluoro-2-(5-fluoropyridin-2-yl)acetamido)benzamide (580 mg, 1.87 mmol) were added dichloroethane (15 mL) and TEA (11 mL, 75 mmol) followed by chlorotrimethylsilane (3.56 mL, 28 mmol) and the mixture was heated at 85° C. for 2-3 h. The mixture was concentrated to dryness and the residue was partitioned between saturated aq ammonium chloride and EtOAc. The organic layer was concentrated and the residue was purified by silica gel chromotography eluting with 0-10% MeOH/DCM to afford 2-(difluoro(5-fluoropyridin-2-yl)methyl)quinazolin-4-ol as a solid (500 mg, 91%). LC-MS (ESI) m/z 292 (M+H)+.

1. concentrationThe mixture was concentrated to dryness
2. customthe residue was partitioned between saturated aq ammonium chloride and EtOAc
3. concentrationThe organic layer was concentrated
4. customthe residue was purified by silica gel chromotography
5. washeluting with 0-10% MeOH/DCM