反应详情

温度

75 °C

A mixture of 2-((3-fluoro-4-nitrophenoxy)methyl)-5-methylpyridine (1.50 g, 5.72 mmol), 4-bromo-2-fluorobenzylamine hydrochloride (1.51 g, 6.29 mmol), DIPEA (2.96 mL, 17.2 mmol) and acetonitrile (19.1 mL) was sealed in reaction vessel and heated to 75° Celsius for 18 h. The mixture was then cooled to RT, transferred to a round bottomed flask and concentrated to dryness. The resulting residue was then heated in a minimum amount of i-PrOH to 70° Celsius until homogeneous. The resulting solution was then cooled to RT where yellow solids precipitated, which were collected by filtration. (2.40 g, 94%). MS (ESI): mass calcd. for C20H17BrFN3O3, 445.04; m/z found, 446.0 [M+H]+.

1. customwas sealed in reaction vessel
2. temperatureThe mixture was then cooled to RT
3. customtransferred to a round bottomed flask
4. concentrationconcentrated to dryness
5. temperatureThe resulting residue was then heated in a minimum amount of i-PrOH to 70° Celsius until homogeneous
6. temperatureThe resulting solution was then cooled to RT where yellow solids
7. customprecipitated
8. filtrationwhich were collected by filtration