Lithium Hydroxide → HCID 117840608, compound

Participants

Reaction Steps

To a solution of the crude N-(3-((4-((3R)-3-cyano-3-ethyl-2-oxopyrrolidin-1-yl)pyrimidin-2-yl)amino)phenyl)-N-(methylsulfonyl)methanesulfonamide (100 mg) in tetrahydrofuran (3.0 mL) was added 4 M aqueous lithium hydroxide solution (52 μL), and the mixture was stirred at room temperature for 3 hr. To the reaction mixture was added saturated aqueous ammonium chloride solution, and the mixture was extracted with ethyl acetate. The obtained organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate). To a solution of the residue in ethanol (3.0 mL) was added 1 N hydrochloric acid (72 μL), and the mixture was stirred at room temperature for 5 min. The solvent was evaporated under reduced pressure, and the residue was recrystallized (ethanol/diisopropyl ether) to give the title compound (12 mg).

Provenance & Evidence