反应详情

温度

105 °C

POCl3 (275 mg, 1.8 mmol) was added to 1 ml DMF at ambient temperature and stirred for 30 minutes. The product of Step 1, above (2) (208 mg, 0.93 mmol), was dissolved in 1 ml DMF, added to the reaction mixture and stirred for 1 hour at ambient temperature. The reaction mixture was heated to 105° C. for 3 hours, cooled to ambient temperature, quenched with saturated sodium acetate solution and extracted (2×10 ml, EtOAc). The organics were washed with brine and dried over MgSO4, filtered and concentrated to yield the title compound (3).

1. additionadded to the reaction mixture
2. stirringstirred for 1 hour at ambient temperature
3. temperaturecooled to ambient temperature
4. customquenched with saturated sodium acetate solution
5. extractionextracted (2×10 ml, EtOAc)
6. washThe organics were washed with brine
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated