反应详情

HATU (0.057 g, 0.15 mmol) was added to a solution of 3-{[3-(aminomethyl)-6-chloro-2-fluorophenyl]oxy}-5-chlorobenzonitrile (0.047 g, 0.15 mmol), 3-chloro-5-(2-hydroxyethyl)-1H-pyrrole-2-carboxylic acid (0.028 g, 0.15 mmol) and DIPEA (0.026 mL, 0.150 mmol) in DMF (2 mL). The resulting solution was stirred for 2 hours then partitioned between water and EtOAc. The organic layer was separated, dried over MgSO4 and evaporated to a residue. The residue was purified by reverse-phase HPLC (water/acetonitrile with 0.1% TFA) to afford the title compound (0.0016 g, 2%) as a film. 1H NMR (400 MHz, Acetone-d6) δ ppm 7.60-7.68 (m, 1H), 7.48-7.53 (m, 1H), 7.41-7.45 (m, 2H), 7.37-7.40 (m, 2H), 6.03 (d, 1H), 4.69 (d, 2H), 3.78 (t, 2 H), 2.82 (t, 2H). LCMS: m/z=479.9 (M−1).

1. customthen partitioned between water and EtOAc
2. customThe organic layer was separated
3. dry with materialdried over MgSO4
4. customevaporated to a residue
5. customThe residue was purified by reverse-phase HPLC (water/acetonitrile with 0.1% TFA)