反应详情

温度

100 °C

2,3,6-trifluoropyridine (1.07 mL, 1.5 g, 11.27 mmol), 3-fluorobenzylamine (3.18 mL, 3.53 g, 28.2 mmol), and triethylamine (4.71 mL, 3.42 g, 33.8 mmol) were dissolved in NMP (39 mL) to form a mixture This mixture reaction mixture was stirred at 100° C. for 1 hr. The reaction mixture was then extracted with EtOAc (3×75 mL). The combined extracts were washed with H2O (4×75 mL) followed by brine (1×75 mL). The organic layer was dried (Na2SO4), filtered, and the solvent removed in vacuo. The resulting residue was subjected to silica gel column chromatography. Elution using 100 hexanes to 30 EtOAc/70 hexanes yielded 2.63 g (98%) of 3,6-difluoro-N-(3-fluorobenzyl)pyridine-2-amine. LCMS (m/z): 239.1 (MH+), retention time=1.01 min.

1. customto form a mixture
2. customThis mixture reaction mixture
3. extractionThe reaction mixture was then extracted with EtOAc (3×75 mL)
4. washThe combined extracts were washed with H2O (4×75 mL)
5. dry with materialThe organic layer was dried (Na2SO4)
6. filtrationfiltered
7. customthe solvent removed in vacuo
8. washElution