反应详情

温度

50 °C

The crude methyl 2-(4-fluorophenyl)imidazo[1,2-a]pyrazine-8-carboxylate (35.7 g, 65.8 mmol) was dissolved in 1,4-dioxane (200 mL), then water (20.2 mL) and lithium hydroxide monohydrate (27.6 g, 658 mmol) were added. Heated to about 50° C. overnight. The reaction mixture was cooled to ambient temperature, filtered, and the collected solid was washed with Et2O (4×70 mL). The resulting brown solid was suspended in water (200 mL) and the pH was adjusted to ˜5 with glacial HOAc (100 mL). The solid was collected, washed with water (4×75 mL) and Et2O (2×80 mL) to give the wet crude title compound (26.4 g, 156%) that was carried on without further purification. LC/MS (Table 1, Method b) Rt=1.21 min; MS m/z: 258.2 (M+H)+.

1. temperatureThe reaction mixture was cooled to ambient temperature
2. filtrationfiltered
3. washthe collected solid was washed with Et2O (4×70 mL)
4. customThe solid was collected
5. washwashed with water (4×75 mL) and Et2O (2×80 mL)