Aluminium lithium hydride → HCID 22221614, compound

Participants

Reaction Steps

To a cooled (0° C) solution of 119 (0.18 g, 0.58 mmol) in THF (10 ml) was added LiAlH4 (1.5 ml of 1.0M in THF) dropwise. After stirring for 30 min, the reaction was quenched with 2N HCl and partitioned between 2N HCl and EtOAc. The EtOAc was separated, dried, and concentrated. The product was purified by column chromatography on silica gel (30% EtOAc/Hex) to give 120 as a yellow solid (0.075 g, 51%); Mp=261-263° C.; 1H NMR (DMSO-d6) δ 10.36 (s,1 H), 9.79 (s, 1 H), 9.77 (s, 1 H), 7.76 (d, 2 H, J=8.5 Hz), 7.25 (d, 1 H, J=2.0 Hz), 7.17 (s, 1 H), 7.12 (d, 1 H, J=2.1 Hz), 6.88 (d, 2 H, J=8.5 Hz); MS 255 (M+H)+

Provenance & Evidence