反应详情

温度

100 °C

To a microwave vial was added N′-(2-hydroxy-3-phenylpyrido[2,3-b]pyrazin-6-yl)pyrazine-2-carbohydrazide (8-4, 0.412 g, 1.147 mmol), MeCN (5.0 mL), and finally phosphorus oxychloride (0.687 mL, 7.37 mmol). The reaction mixture was then heated to 100° C. in a hot oil bath (capped) overnight. The reaction mixture was then permitted to cool to room temperature, diluted with MeCN & concentrated in vacuo. The resulting residue was then suspended in ethyl acetate, washed with a saturated solution of sodium bicarbonate, followed by water, then brine, dried over sodium sulfate, filtered, and concentrated in vacuo to give 8-5 as a brown solid. HRMS (M+H)+: observed=360.0773, calculated=360.0759.

1. custom(capped) overnight
2. temperatureto cool to room temperature
3. concentrationconcentrated in vacuo
4. washwashed with a saturated solution of sodium bicarbonate
5. dry with materialbrine, dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated in vacuo