反应详情

温度

100 °C

To a flask was added 6-chloro-3-phenylpyrido[2,3-b]pyrazin-2-ol (8-2, 3.41 g, 13.23 mmol), anhydrous hydrazine (5.0 mL, 159 mmol), and finally 1.4 Dioxane (60 mL). The stirred reaction mixture was then heated to 100° C. in a hot oil bath under an atmosphere of nitrogen with an air cooled reflux condenser attached. Upon completion of the reaction the mixture was cooled to room temperature, suspended in ethyl acetate and washed with a saturated solution of sodium bicarbonate, followed by water, then brine, dried over sodium sulfate, filtered, and concentrated in vacuo to give 8-3 as an orange/tan foam. HRMS (M+H)+: observed=254.1041, calculated=254.1037.

1. customThe stirred reaction mixture
2. temperaturecooled
3. temperaturereflux condenser
4. customUpon completion of the reaction the mixture
5. temperaturewas cooled to room temperature
6. washwashed with a saturated solution of sodium bicarbonate
7. dry with materialbrine, dried over sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated in vacuo