反应详情

A solution of (5-methylthiophen-2-yl)-oxo-acetic acid ethyl ester (5.5 g, 28 mmol) in THF (20 ml), water (20 ml), and 50% NaOH (4 ml) was stirred under reflux for 18 hours. The reaction mixture was allowed to cool to ambient temperature. After partial evaporation, the reaction mixture was acidified with 1N HCl and extracted with diethyl ether (2×50 ml). The organic layer was dried over sodium sulfate and concentrated under vacuum to yield (5-methylthiophen-2-yl)-oxo-acetic acid (4.8 g, 100%). 1H NMR (300 MHz, CDCl3) δ8.40 (1H, d, J=4.0 Hz), 6.95 (1H, d, J=3.9 Hz), 2.63 (3H, s).

1. temperatureunder reflux for 18 hours
2. customAfter partial evaporation
3. extractionextracted with diethyl ether (2×50 ml)
4. dry with materialThe organic layer was dried over sodium sulfate
5. concentrationconcentrated under vacuum