Lithium hydroxide, monohydrate → HCID 90386883, compound

Participants

Reaction Conditions

Reaction Steps

A solution of Example 93e (3.36 g, 10.29 mmol) and lithium hydroxide monohydrate (3.17 g, 76 mmol) in ethanol (47.5 mL) and water (2.5 mL) was added to 100 mL microwave reaction vessel with stir bar. The mixture was heated at 120° C. for 30 minutes in a Ethos Microsynth multimode microwave reactor (Milestone Inc.), then cooled to ambient temperature. The reaction mixture was added to 200 mL water and stirred for 15 minutes. The mixture extracted with 3×200 mL 10% methanol/dichloromethane and the combined dichloromethane extracts dried over anhydrous sodium sulfate. Filtration and solvent removal provided a brown oil which was chromatographed on a 40 g silica cartridge eluting with 0-10% methanol/dichloromethane to provide the title compound.

Provenance & Evidence