Potassium Hydroxide → HCID 12226278, compound

Participants

Reaction Steps

Potassium hydroxide pellets (58.6 g) was slowly added to a solution of the product (85.0 g) from step (j) dissolved in 1 L of methanol/THF (1:1). After refluxing for 3 hours, the reaction mixture was cooled to room temperature and concentrated in vacuo. The resulting residue was triturated with 1N HCl then extracted with EtOAc. The organic layer was separated, washed with 2×250 ml of 1N HCl then washed with 3×400 ml of 1N NaOH. The aqueous basic layers were combined and acidified with conc. HCl to afford the title product (54.8 g) as a gold solid. 1H NMR was consistent with the proposed structure.

Provenance & Evidence