Dimethylformamide → HCID 57551776, compound

Participants

Reaction Steps

DMF (10 mL) was cooled in an ice bath and phosphorus oxychloride (0.40 mL) was added over 20 seconds. The solution was stirred for 10 minutes at room temperature and then the product of step i) (0.6 g) in DMF (2 mL) was added over 5 minutes. The mixture was heated at 80° C. overnight. The mixture was allowed to cool then poured onto ice/water and stirred for 20 minutes. The aqueous was extracted with ethyl acetate, the organics were combined and evaporated under reduced pressure. The residue was purified (SiO2, eluting with 1:4 ethyl acetate:isohexane) to give the sub-title compound (0.4 g).

Provenance & Evidence