反应详情

温度

100 °C

A mixture of 5-bromopyrazine-2,3-diamine (50 mg, 0.3 mmol) and ethyl 2-cyclopropylpyrimidine-4-carbimidate (Intermediate 19, 50.7 mg, 0.3 mmol), triethylamine (73.8 μL, 0.5 mmol), acetic acid (244 μL, 4.2 mmol) and ethanol (0.8 mL) was heated to 100° C. for 30 min. The mixture was concentrated and diluted with water. Then a saturated aqueous solution of sodium bicarbonate was added and the mixture was extracted with ethyl acetate. The organics were washed with brine, dried over sodium sulfate, and concentrated under reduced pressure. The crude material was purified via flash chromatography (0-5% methanol in dichloromethane) to afford 6-bromo-2-(2-cyclopropylpyrimidin-4-yl)-1H-imidazo[4,5-b]pyrazine (21 mg, 25%).

1. concentrationThe mixture was concentrated
2. additiondiluted with water
3. additionThen a saturated aqueous solution of sodium bicarbonate was added
4. extractionthe mixture was extracted with ethyl acetate
5. washThe organics were washed with brine
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe crude material was purified via flash chromatography (0-5% methanol in dichloromethane)