反应详情

温度

110 °C

A mixture of N-[(1S,2S)-2-aminocyclopentyl]-2-(2H-1,2,3-triazol-2-yl)benzamide hydrochloride (Intermediate 4; 75 mg, 0.24 mmol), 2-bromo-5-(trifluoromethoxy)pyridine (CAS number 888327-36-4; 59 mg, 0.24 mmol), BINAP (15 mg, 0.024 mmol), tris(dibenzylideneacetone)dipalladium(0) (11 mg, 0.012 mmol) and sodium tert-butoxide (33 mg, 0.34 mmol) in dry toluene (2.4 ml) was sealed, evacuated and purged with nitrogen and heated at 110° C. for 17 hours. The reaction was partitioned between ethyl acetate and water, washing with water, brine, filtered through a hydrophobic frit and concentrated in vacuo. The residue was purified by column chromatography (silica, 0-100% ethyl acetate/petrol) to afford the title compound.

1. customwas sealed
2. customevacuated
3. custompurged with nitrogen
4. customThe reaction was partitioned between ethyl acetate and water
5. washwashing with water, brine
6. filtrationfiltered through a hydrophobic frit
7. concentrationconcentrated in vacuo
8. customThe residue was purified by column chromatography (silica, 0-100% ethyl acetate/petrol)