1,2-Dichloroethane → HCID 66678340, compound

Participants

Reaction Steps

To a solution of Intermediate 76 (0.148 g, 0.45 mmol) and Intermediate 5 (0.107 mg, 0.375 mmol) in ACN (2.5 mL) was added EDC (0.101 g, 0.53 mmol). The reaction mixture was stirred at room temperature for 18 hours. The reaction mixture was diluted with pyridine (2.5 mL) and heated at 150° C. in the microwave for 30 minutes. The solvent was removed in vacuo and the residue dissolved in DCM. The mixture was washed with water and the organic phase passed through a hydrophobic frit. The solvent was evaporated in vacuo. The residue was purified by flash chromatography (silica, iso-hexane/EtOAc) to afford the title compound. 1H NMR (CDCl3, 400 MHz) δ 8.62 (1H, d, J=1.7 Hz), 8.39 (1H, dd, J=8.0, 1.7 Hz), 7.76 (2H, d, J=7.1 Hz), 7.49 (1H, d, J=8.0 Hz), 7.38-7.22 (3H, m), 7.15 (1H, d, J=7.6 Hz), 3.99 (2H, s), 3.25 (2H, s), 2.45 (3H, s), 2.07 (3H, s), 1.50 (9H, s).

Provenance & Evidence