Water → HCID 12043734, compound

Participants

Reaction Steps

To a solution of Compound 20 (0.41 g, 1.1 mmol) obtained in Example 19 in ethanol (4.1 mL) was added a 2 mol/L aqueous solution of sodium hydroxide (1.1 mL), and the mixture was stirred at room temperature for 1 hour and then stirred at 60° C. for 20 minutes. The mixture was allowed to cool, and water and ethyl acetate were added to the mixture, followed by separating into an organic layer and an aqueous layer. The aqueous layer was acidified with 6 mol/L aqueous hydrochloric acid and extracted with ethyl acetate, and the extract was washed with brine and dried over sodium sulfate. The solvent was evaporated in vacuo, toluene was added to the residue, and the mixture was evaporated in vacuo. To the residue was added diisopropyl ether, and the precipitated solid was collected by filtration and recrystallized from ethanol to give Compound 21 (0.13 g, 36%) as a mixture of isomers in white crystals.

Provenance & Evidence