反应详情

5-Isopropylpyrrolo[2,1-f][1,2,4]triazin-4 (3H)-one (0.035 g, 0.198 mmol, 1.0 equiv) was added to phosphorous oxychloride (2.0 ml, 21.5 mmol, 109 equiv) under a nitrogen atmosphere. The reaction mixture was heated to reflux for 1.5 h. The mixture was cooled to room temperature then concentrated in vacuo. The residue was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate. The aqueous layer was extracted twice with ethyl acetate. The combined organic washes were dried over anhydrous magnesium sulfate and concentrated in vacuo to yield a tan solid that was used in the next step without further purification. MS(ESI+) m/z 196 (M+H)+.

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 1.5 h
3. concentrationthen concentrated in vacuo
4. customThe residue was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate
5. extractionThe aqueous layer was extracted twice with ethyl acetate
6. dry with materialThe combined organic washes were dried over anhydrous magnesium sulfate
7. concentrationconcentrated in vacuo
8. customto yield a tan solid that
9. customwas used in the next step without further purification