Hydrogen chloride-ethyl acetate → HCID 67442257, compound

Participants

Reaction Steps

To a suspension of 270 (996 mg, 1.90 mmol) in EtOAc (20 mL) was added 1N HCl-EtOAc (11.4 mL, 11.4 mmol). The reaction mixture was stirred for 18 hours, the precipitate was collected by filtration, washed with EtOAc (30 mL) and dried to afford title compound 271 (962 mg, 100% yield) as a pale yellow solid. 1H NMR (300 MHz, DMSO-d6) δ (ppm): 9.22 (br, 2H), 9.03 (s, 1H), 8.58 (d, J=6.0 Hz, 1H), 7.74 (dd, J=13.5, 2.7 Hz, 1H), 7.70 (s, 1H), 7.38 (t, =9.0 Hz, 1H), 7.25-7.15 (m, 1H), 6.77 (d, J=6.0 Hz, 1H), 6.72 (s, 1H), 6.47 (s, 1H), 4.80-4.30 (br, 1H), 3.85-3.75 (m, 2H), 3.42-3.31 (m, 2H), 2.90-2.80 (m, 2H), 2.60-2.40 (m, 1H), 0.70-0.60 (m, 2H), 0.48-0.35 (m, 2H).

Provenance & Evidence