Aluminium lithium hydride → HCID 117689132, compound

Participants

Reaction Steps

A 1N THF solution of LAH (0.175 mL, 0.175 mmol) was added dropwise to a 0° C. solution of ethyl-4-{[(1S,2S)-2-(5-methoxypyridin-2-yl)cyclopropyl]methoxy}-2-methylpyrimidine-5-carboxylate (30 mg, 0.087 mmol) in THF (0.58 mL). The reaction mixture was slowly warmed to room temperature, and then stirred for 30 mins. The reaction mixture was re-cooled to 0° C. and the carefully quenched by dropwise addition of water (10 μL), 15% NaOH in water (20 μL), and then water (20 μL). The slurry was treated with excess Na2SO4, stirred vigorously at room temperature for 10 mins, and then filtered through a pad of Celite eluting exhaustively with 1:1 CH2Cl2/MeOH. The filtrated was concentrated in vacuo. The resulting product was sufficiently pure to use in the subsequent step without further purification. LRMS m/z (M+H) 302.4 found, 302.1 required.

Provenance & Evidence