反应详情

温度

80 °C

To a solution of 4-benzyloxy-2-fluoro-benzaldehyde (1.3 g, 5.6 mmol) in DMSO (55 mL) was added mercapto-acetic acid methyl ester (1.2 mL, 11.3 mmol) and Et3N (2.4 mL, 1.7 g, 16.8 mmol) and the reaction mixture was heated (80° C., 12 h). The reaction mixture was cooled (rt), treated with H2O (100 mL) and filtered. The resulting residue was purified by silica gel flash chromatography using EtOAc:hexane (0-30%) to provide the title compound as yellow solid (1.6 g, 96%). MS (ESI): mass calcd. for C17H14O3S, 298.1; m/z found, 299.1 [M+H]+. 1H NMR (500 MHz, CDCl3): 7.98 (s, 1H), 7.75 (d, J=8.8, 1H), 7.53-7.30 (m, 6H), 7.10 (dd, J=8.8, 2.3, 1H), 5.14 (s, 2H), 3.92 (s, 3H).

1. temperatureThe reaction mixture was cooled (rt)
2. filtrationfiltered
3. customThe resulting residue was purified by silica gel flash chromatography