反应详情

温度

100 °C

To a suspension of amide 1 (9.6 g, 26 mmol) in anhydrous 1,4-dioxane (100 mL) was added phosphorous oxychloride (POCl3) (9.2 mL, 100 mmol) slowly. The whole was then heated at 100° C. overnight. After cooling to r.t., the mixture was poured into ice (200 g) with stirring. Filtration, followed by recrystallization in DCM/hexanes gave a pale grey solid (Compound 5) (8.2 g, in 90% yield).

1. temperatureAfter cooling to r.t.
2. filtrationFiltration
3. customfollowed by recrystallization in DCM/hexanes