Acetic Acid Mixture with Hydrobromic Acid → HCID 178515741, compound

Participants

Reaction Steps

A 3-necked roundbottom flask, was charged with (E)-ethyl 3-(5-amino-2-iodopyrimidin-4-yl)acrylate (120 g, 388 mmol) followed by hydrogen bromide/acetic acid (1500 ml). The resulting solution was allowed to react, with stirring, for 1.5 hours while the temperature was maintained at 40˜50° C. Upon completion, the mixture was concentrated under reduced pressure. The resulting residue was dissolved in 500 ml of methanol and the pH was adjusted to 7 by the addition of sodium bicarbonate. The resulting mixture was washed once with a solution of 46 g of NaHSO3 in 200 mL of water. The organic layer was concentrated under reduced pressure. The resulting slurry was filtered and the solids collected to afford the title compound.

Provenance & Evidence