反应详情

温度

140 °C

The methoxy derivative, Compound 3.2 (14.54 g, 70 mmol), was dissolved in iodine free hydriodic acid (150 mL) and refluxed at 140° C. for four hours. After the resulting brown solution was cooled to room temperature, water was added and the mixture was neutralized. The aqueous phase was then washed with ether; the organic layers were combined, decolorized, dried and evaporated. The remaining residue was purified by flash silica chromatography to yield a white solid (11.93 g, 88%). 1 H NMR (CDCl3) δ8.20 (d, 2H), 7.02 (d, 2H), 3.32 (t, 2H), 2.88 (d, 2H).

1. temperatureAfter the resulting brown solution was cooled to room temperature
2. washThe aqueous phase was then washed with ether
3. customdried
4. customevaporated
5. customThe remaining residue was purified by flash silica chromatography