Aluminium lithium hydride → HCID 66972054, compound

Participants

Reaction Conditions

Reaction Steps

A round-bottom flask containing the product of Step 1 (1.94 g, 3.88 mmol) was fitted with a condenser, stirbar and septa and flushed with nitrogen. Tetrahydrofuran (40 mL) was added, giving a solution that was cooled to 0° C. Lithium aluminum hydride (0.77 g, 20 mmol) was added, and the reaction was then removed from the cooling bath and allowed to warm to room temperature. After one hour, the reaction was warmed to 60° C., then stirred an additional 17 hours. The reaction mixture was then cooled to room temperature and quenched via the sequential additions of H2O (0.77 mL), 10% aqueous sodium hydroxide solution (0.77 mL), and H2O (3×0.77 mL). The resulting mixture was stirred 10 minutes, diluted with ethyl acetate (100 mL), filtered through celite and concentrated in vacuo to give the desired product.

Provenance & Evidence