Hydrochloric Acid → HCID 21844867, compound

Participants

Reaction Conditions

Reaction Steps

In a 250 mL RB flask, the compound of Example 13 (1.0 g, 1.5 mmol) is dissolved in ethanol (30 mL) and water is added until the solution turns slightly turbid. The reaction mixture is heated at 100° C. and 1N LiOH (12 mL) is added. After maintaining the mixture at 100° C. for 8 hours, the solution is adjusted to pH 0.5 with 5N HCl (aq), and the mixture is refluxed for 1.5 hours and stirred at ambient temperature for an additional 18 hours. The cooled reaction material is desalted by ion exchange chromatography using an AG5OW-X8 [80 mL, (H+ form)] strongly cation exchange resin. The product is eluted with 1.0N NH4OH. The fractions containing product are combined and concentrated to afford the title compound.

Provenance & Evidence