反应详情

To a solution of N-((5-bromopyridin-2-yl)methyl)acetamide (450 mg, 1.96 mmol) in toluene (15 mL) was added POCl3 (600 mg, 3.92 mmol) and the mixture stirred at refluxing temperature for 6 h. After cooling, the reaction mixture was quenched by adding water (1 mL) and concentrated to remove toluene. The residue was diluted with water (5 mL) and extracted with EtOAc (3×10 mL) with the organic layer concentrated to give a crude product which was used in next step without further purification (290 mg, Yield 70%). LCMS (m/z): 211.0 (M+1)

1. temperatureat refluxing temperature for 6 h
2. temperatureAfter cooling
3. customthe reaction mixture was quenched
4. additionby adding water (1 mL)
5. concentrationconcentrated
6. customto remove toluene
7. additionThe residue was diluted with water (5 mL)
8. extractionextracted with EtOAc (3×10 mL) with the organic layer
9. concentrationconcentrated