Sodium Hydroxide → HCID 20244036, compound

Participants

Reaction Steps

To a solution of a total amount of the hydrochloride in 80 ml of methanol was added a solution of 2 g of sodium hydroxide in 10 ml of water, and the mixture was stirred for 10 minutes. After the methanol was concentrated, water was added to the residue to separate oil. To the oil was added 3 ml of glacial acetic acid and ethyl acetate, and the mixture was shaken well. The organic layer was washed with water and an aqueous solution of sodium hydrogencarbonate and the precipitated crystals were filtered. The crystals were dissolved in acetone containing ethanol and treated with concentrated hydrochloric acid to precipitate the corresponding hydrochloride. The crystalline hydrochloride was filtered and recrystallized from aqueous ethanol to give 5-hydroxy-1-isopropyl-2-methyl-N-(1-(2-phenylethyl)-4-piperidyl)indole-3-carboxamide hydrochloride, melting at 271°-276° C. with decomposition.

Provenance & Evidence