反应详情

温度

30 °C

3-(Dimethylamino)propan-1-ol (3.09 g, 29.95 mmol) was added to a mixture of sodium hydride (2.4 g, 60.00 mmol) in DMF (50 mL) over a period of 20 min at r.t. 5-Bromo-2-fluoropyridine (5.81, g, 33.01 mmol) was added and the resulting solution stirred for 4 h at 30° C. The reaction was then quenched by the addition of a sat. aqueous solution of ammonium chloride and the resulting mixture concentrated under vacuum. The residue was purified by FCC, eluting with DCM/MeOH in Et2O (10:1) to afford the desired material (5.2 g, 67%) as yellow oil. Mass Spectrum: m/z (ES+)[M+H]+=259.

1. customThe reaction was then quenched by the addition of a sat. aqueous solution of ammonium chloride
2. concentrationthe resulting mixture concentrated under vacuum
3. customThe residue was purified by FCC
4. washeluting with DCM/MeOH in Et2O (10:1)