Hydrochloric Acid → HCID 15684577, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 2-[2-{3-hydroxy-4-(3-methylureido)phenyl}ethyl]-7-methoxy-3-methylimidazo[1,2-a]pyridine (1.9 g) and polyphosphate ester (15 g) was stirred for 1.5 hours at 130° C. To the reaction mixture was added a mixture of ethyl acetate and water, and the mixture was adjusted to pH 1 with 6N hydrochloric acid. The separated aqueous layer was adjusted to pH 8 with aqueous potassium carbonate solution. The aqueous mixture was extracted with a mixture of ethyl acetate and tetrahydrofuran with salting-out technique. The extract was washed with brine and dried over magnesium sulfate. Evaporation of the solvent gave a residue, which was triturated with a mixture of diethyl ether and ethyl acetate, and the resulting precipitate was crystallized from a mixture of methanol, ethyl acetate and isopropyl ether to give 6-[2-(7-methoxy-3-methylimidazo[1,2-a]pyridin-2-yl)ethyl]-2-methylaminobenzoxazole (0.26 g).

Provenance & Evidence