Aluminum(III) Chloride → HCID 58303977, compound

Participants

Reaction Steps

To a solution of LiAlH4 (5 mg, 0.12 mmol) and AlCl3 (16 mg, 0.12 mmol) in THF (5 mL) was added a solution of 30-14 (14 mg, 0.04 mmol) in THF (5 mL) dropwise, the mixture was stirred at room temperature overnight before Na2SO4.10H2O was added. The mixture was filtered and the filtrate was evaporated to give a crude product which was purified by preparative HPLC (acid condition, water/CH3CN, 25-30% CH3CN in 7.5 min, RT=6.5 min) to afford 30-15 (8 mg, 61%) as a yellow solid. 1H-NMR (400 MHz, CDCl3): δ (ppm) 7.30-7.28 (m, 5H), 7.00-6.95 (m, 1H), 6.87-6.84 (m, 2H), 4.24 (q, J=7.2 Hz, 2H), 4.01-3.98 (br.s, 2H), 3.67 (s, 3H), 3.27-3.22 (br.s, 2H), 3.15-3.11 (br.s, 2H), 1.34 (t, J=6.8 Hz, 3H). LRMS: calc 326.2 and found: 327.0 [M+1].

Provenance & Evidence