反应详情

温度

120 °C

A mixture of 4,4,4-trifluoro-3-(2-iodo-5-methoxy-phenylamino)-but-2-enoic acid ethyl ester 76c (0.5 g, 1.2 mmole), Pd(OAc)2 (22.4 mg, 0.1 mmole), PPh3 (52.5 mg, 0.2 mmole) and NaHCO3 (505 mg, 6 mmole) in 5 ml DMF was heated at 120° C. under argon for 24 hours and cooled to room temperature. The mixture was poured into EtOAc/water and washed with brine. The organic layer was dried over Na2SO4 and concentrated under rot vap. The residue was purified by column chromatography to give 217 mg product (63% yield). 1H NMR. (300 MHz, CD3OD) δ 8.00 (1H, d, J=9.0 Hz), 6.96 (1H, d, J=2.0 Hz), 6.90 (1H, dd, J=2.0, 9.0 Hz), 4.37 (2H, m), 3.84 (3H, s), 1.40 (3H, m).

1. temperaturecooled to room temperature
2. washwashed with brine
3. dry with materialThe organic layer was dried over Na2SO4
4. concentrationconcentrated under rot vap
5. customThe residue was purified by column chromatography