Aluminium lithium hydride → HCID 58303925, compound

Participants

Reaction Steps

To a solution of 27-2 (150 mg, 0.42 mmol) in anhydrous THF (20 mL) was added LiAlH4 (78 mg, 2.05 mmol) and the mixture was stirred at room temperature for two hours. Na2SO4.10H2O was added, the solid was filtered off and washed with ethylacetate (20 mL). The filtrate was concentrated in under vacuum. The resulting residue was purified by column chromatographyon (DCM:MeOH=50:1) to afford compound 27-3 (30 mg, 23%) as a white solid. 1H-NMR (400 MHz, MeOD-d6): δ (ppm) 7.02 (s, 1H), 6.65 (d, J=13.2 Hz, 1H), 4.16 (q, J=6.8 Hz, 2H), 3.72 (s, 3H), 3.51 (t, J=6.6 Hz, 2H), 3.22-3.17 (m, 2H), 3.10-3.03 (m, 2H), 2.74 (s, 6H), 2.72-2.64 (m, 2H), 1.79-1.72 (m, 2H), 1.30 (t, J=7.2 Hz, 3H). LRMS: calc 322.4 and found: 323.0 [MH]+.

Provenance & Evidence