反应详情

A mixture of B2, NaOAc (2 eq) and AcOH (0.16 M) was heated at reflux for 4 h. The reaction mixture was cooled down to RT and concentrated under reduced pressure. The crude was purified by preparative RP-HPLC, using H2O (0.1% TFA) and MeCN (0.1% TFA) as eluents (column: Water X-Terra C18). The pooled product fractions were lyophilized to give the title compound. 1H NMR (600 MHz, DMSO-d6) δ: 12.80 (1H, m), 8.84 (2H, s), 7.38-7.28 (3H, m), 6.66 (1H, s), 4.01 (2H, s), 3.85-3.7 (2H, m), 3.55 (1H, m), 3.36-3.32 (2H, m), 3.27 (1H, m), 3.20 (1H, m), 3.16 (1H, m), 2.45-2.42 (2H, m), 2.06 (1H, m), 1.90 (1H, m), 1.11-1.07 (3H, m). MS (ES) C19H23FN4O2 required: 358. found: 359 (M+H)+.

1. temperaturewas heated
2. temperatureat reflux for 4 h
3. concentrationconcentrated under reduced pressure
4. customThe crude was purified by preparative RP-HPLC