反应详情

温度

110 °C

N-(5-(4-methyl-2-propyl-1H-imidazol-1-yl)thiazol-4-yl)acetamide from example 2.5 (8 mg, 0.030 mmol) and phosphorus pentoxide (21.48 mg, 0.15 mmol) were added sequentially quickly to POCl3 (5 mL). The mixture was heated to 110° C. for 4 h, POCl3 was evaporated and the residue was quenched with ice-water. The mixture was neutralized with saturated Na2CO3 solution and extracted with EA (3×20 mL). The combined organic layer was washed with brine and concentrated to give brown liquid. It was purified by pre-HPLC to give the title compound (5.0 mg, 0.02 mmol, 67.1%) as a white solid.

1. customPOCl3 was evaporated
2. customthe residue was quenched with ice-water
3. extractionextracted with EA (3×20 mL)
4. washThe combined organic layer was washed with brine
5. concentrationconcentrated
6. customto give brown liquid
7. customIt was purified by pre-HPLC