反应详情

To a suspension of isonicotinic acid hydrochloride (1.48 g, 10.0 mmol, 1.2 equiv) in DMF was added EDC (3.90 g, 2.0 equiv), HOBt (2.7 g, 2.0 equiv) and NEt3 (3.03 g, 3.0 equiv). After being stirred at room temperature for 1.0 h, the solution was added with 4-(2-aminothiazol-4-yl)-3,5-dimethylphenol (5-2, 2.2 g, 1.0 equiv). The reaction mixture was stirred at room temperature overnight. The solution was concentrated and the residue was re-dissolved in EtOAc. The solution was washed with brine, dried over MgSO4, and concentrated under reduced pressure to give brown solid. The brown solid was washed with 50% EtOAc in hexanes to give 5-3 (2.08 g) as white solids in 64% yield: 1H NMR (500 MHz, CDCl3) δ 9.29 (s, 1 H), 8.80 (d, 2 H), 7.98 (d, 2 H), 7.06 (s, 1 H), 6.51 (s, 2 H), 2.01 (s, 6H).

1. stirringThe reaction mixture was stirred at room temperature overnight
2. concentrationThe solution was concentrated
3. dissolutionthe residue was re-dissolved in EtOAc
4. washThe solution was washed with brine
5. dry with materialdried over MgSO4
6. concentrationconcentrated under reduced pressure
7. customto give brown solid
8. washThe brown solid was washed with 50% EtOAc in hexanes