Trifluoroacetic acid → HCID 53864767, compound

Participants

Reaction Steps

A solution of Intermediate 5 (12.46 g) in dichloromethane (124 ml) at 0° C. was treated dropwise with neat trifluoroacetic acid (120 ml). The resulting pale yellow solution was allowed to reach room temperature over 48 h. The solvent was subsequently removed and the crude product dissolved in the minimum volume of 1N hydrochloric acid at 0° C. The aqueous phase was extracted with dichloromethane to remove any impurities. The aqueous phase was then taken to pH 8.5, initially using solid sodium bicarbonate and then a few drops of 3N sodium hydroxide. A white precipitate formed which was filtered, and the residue washed with water and dried in vacuo (7.2 g 83%). TLC Rf 0.10 (EtOAc).

Provenance & Evidence