反应详情

温度

60 °C

A suspension of sodium hydride (2 g, 50.0 mmol) in DMF (20 ml) was cooled to 0 degree before 2-(4-bromophenyl)acetonitrile (4 g, 20.40 mmol) was added slowly, The suspension was stirred at 0 degree for another 10 min before 1,3-dibromo-2,2-dimethoxypropane (2.62 g, 10.00 mmol) was added. The reaction mixture was stirred at 60° C. for 20 h before cooled to room temperature, poured into water (75 ml) and extracted with ethyl acetate (2×50 ml). The combined organic phase was washed with water (75 ml), brine (50 ml) and concentrated. The crude product was purified by column (100 g, biotage) eluted with ethyl acetate/cyclohexane (0-10%) to afford product 1.7 g (59% yield). 1H NMR (500 MHz, DMSO-d6): 7.46 (d, 2H), 7.29 (d, 2H), 3.21 (s, 3H), 3.11 (s, 3H), 3.03 (d, 2H), 2.62 (d, 2H).

1. additionwas added slowly
2. additionwas added
3. temperaturebefore cooled to room temperature
4. extractionextracted with ethyl acetate (2×50 ml)
5. washThe combined organic phase was washed with water (75 ml), brine (50 ml)
6. concentrationconcentrated
7. customThe crude product was purified by column (100 g, biotage)
8. washeluted with ethyl acetate/cyclohexane (0-10%)