反应详情

温度

100 °C

To a flask containing (5-Bromo-thiazol-2-yl)-pyridin-2-yl-amine (5-4, 4.58 g, 17.9 mmol was added 30 mL acetic anhydride. The suspension was then heated to 100° C. After about 1.5 hours, the acetic anhydride and acetic acid was removed under reduced pressure, heating the bath to 70° C. Two 70 mL portions of toluene were also added for azeotropic distillation. The product was obtained as a tan colored precipitate. 1H NMR (DMSO-d6): δ8.65 (d, 1H, J=3.9 Hz), 8.09 (t, 1H, J=8.6 Hz), 7.67 (d, 1H, J=8 Hz), 7.59 (t, 1H, J=6.6 Hz), 7.47 (s, 1H). mp 132-138° C.

1. customthe acetic anhydride and acetic acid was removed under reduced pressure
2. temperatureheating the bath to 70° C
3. additionTwo 70 mL portions of toluene were also added for azeotropic distillation
4. customThe product was obtained as a tan colored precipitate