Water → HCID 118092988, compound

Participants

Reaction Conditions

Reaction Steps

36B (2.609 g, 6.34 mmol) was dissolved in DMSO (40 mL), lithium chloride (0.538 g, 12.68 mmol) and water (0.114 mL, 6.34 mmol) were added. The reaction mixture was stirred at 130° C. for 2 h, then cooled to rt, diluted with EtOAc (250 mL), washed with water (2×100 mL), brine (1×100 mL) and dried (Na2SO4). EtOAc was removed under reduced pressure and the residue was purified by flash chromatography (0-70% EtOAc/hexanes) to give 36C (1.803 g, 5.31 mmol, 84% yield) as a yellowish film. MS (ESI) m/z: 340.1 [M+1]+. 1H NMR: (400 MHz, CDCl3) δ ppm 8.20 (1H, d, J=7.07 Hz), 8.09 (1H, br. s.), 7.67 (1H, d, J=5.05 Hz), 7.29-7.46 (5H, m), 5.19 (2H, s), 4.59 (2H, br. s.), 3.91 (2H, br. s.), 2.94 (3H, br. s.).

Provenance & Evidence