Hydrochloric Acid → BMY-25368 hydrochloride

Participants

Reaction Conditions

Reaction Steps

A mixture of 1-amino-2-[3-(3-piperidinomethylphenoxy)-propylamino]-1-cyclobutene-3,4-dione [prepared in Step A] (2.68 g, 0.0078 mole), 2-propanol (8.5 mL), and 1M aqueous hydrochloric acid (8.0 mL, 0.008 mole) was heated to reflux with stirring. Insoluble material was removed by filtration and acetone (24 mL) was added to the hot solution. The mixture was stirred at ambient temperature for 18 hours, then cooled to 0° C. The solid was collected by filtration, washed with acetone:2-propanol (2:1) (3 mL), and dried in vacuo to give 1.67 g (56.4% yield) of the title compound as an off-white powder. The product was shown by spectral data to be identical to authentic sample of the hydrochloride salt.

Provenance & Evidence