反应详情

温度

80 °C

To a solution of 3-morpholin-4-yl-N-pyridin-2-ylmethyl-propionamide (5.4 g, 21.7 mmol) in 1,2-dichloroethane (100 mL), cooled in an ice bath, was added POCl3 (12 mL). The mixture was heated to 80° C. for 3 h. After this time the mixture was allowed to cool and poured slowly into 10% aqueous potassium carbonate (500 mL). The mixture was extracted with dichloromethane (200 mL) and ethyl acetate (200 mL) and the combined organic layers were dried over anhydrous sodium sulfate and concentrated in vacuo. The residue was chromatographed on silica to yield 3-(2-morpholin-4-yl-ethyl)-imidazo[1,5-a]pyridine (3.89, 78%).

1. temperatureto cool
2. extractionThe mixture was extracted with dichloromethane (200 mL) and ethyl acetate (200 mL)
3. dry with materialthe combined organic layers were dried over anhydrous sodium sulfate
4. concentrationconcentrated in vacuo
5. customThe residue was chromatographed on silica