Example 217
To a solution of Compound 265 (25 mg, 63.8 umol, 1 eq) in DMF (1 mL) at 30° C. was added NaN3 (5.0 mg, 76.6 umol, 1.2 eq). The resulting mixture was stirred at 60° C. for 6 h. The reaction mixture was diluted with water (20 mL) and extracted with EA (20 mL*3). The combined organic layers were washed with brine (20 mL), dried over Na2SO4, filtered and concentrated under reduced pressure to give a residue (containing some DMF). The residue was purified by prep-HPLC (column: Waters Xbridge 150*50 10u; mobile phase: [water (0.05% ammonia hydroxide v/v)-ACN]; B %: 59%-89%, 10 min) to give Compound 256 (15.8 mg, 39.7 umol, 62.3% yield) as a white solid. LCMS (ESI): RT=0.898 min, mass calc. for C21H17F3N4O 398.14, m/z found 399.0 [M+H]+; 1H NMR (400 MHz, CDCl3) δ 8.38 (d, J=1.8 Hz, 1H), 8.00 (d, J=8.3 Hz, 1H), 7.91-7.85 (m, 1H), 7.78 (d, J=7.5 Hz, 3H), 7.65-7.58 (m, 3H), 7.52 (dd, J=1.1, 7.2 Hz, 1H), 6.55 (brs, 1H), 3.64 (q, J=6.5 Hz, 2H), 3.51 (t, J=6.5 Hz, 2H), 1.98 (quin, J=6.5 Hz, 2H).
