反应详情

温度

90 °C

An oven dried flask under N2 was charged with 2 ml of N,N-dimethylformamide and phosphorous oxychloride (0.048 ml, 0.52 mmol) was added dropwise. 7-Phenylimidazo[1,2-a]pyridine (1-4, 0.100 g, 0.515 mmol) was added and the reaction was heated to 90° C. After 4 h additional POCl3 (0.048 ml, 0.52 mmol) was added and the reaction was heated overnight. Another sample of POCl3 (0.048 ml, 0.52 mmol) was added and heating was continued. After 4 h more, the reaction was cooled to ambient temperature. The reaction was quenched with saturated aqueous NaHCO3 and extracted 3× with DCM. The extracts were dried over Na2SO4, filtered and concentrated.

1. customAn oven dried flask under N2
2. additionwas added dropwise
3. temperaturethe reaction was heated overnight
4. temperatureheating
5. temperaturethe reaction was cooled to ambient temperature
6. customThe reaction was quenched with saturated aqueous NaHCO3
7. extractionextracted 3× with DCM
8. dry with materialThe extracts were dried over Na2SO4
9. filtrationfiltered
10. concentrationconcentrated