反应详情

温度

0 °C

To a suspension of Ph3P (1.0 g) in 40 mL of MeCN at 0° C. was added bromine (0.6 g) and the mixture was stirred at 0° C. for 15 minutes and then warmed to ambient temperature. To the suspension of Br2PPh3 was then added 3-cyano-1-(3-hydroxyprop-2-en-1yl)benzene (0.5 g) in 10 mL MeCN dropwise. The resulting solution was stirred at 60° C. for 30 minutes, cooled to ambient temperature and concentrated. The residue was triturated with 10% hexane in ethyl acetate. The mixture was filtered through a silica gel pad and the filtrate was concentrated to afford 0.71 g of 3-cyano-1-(3-bromoprop-2-en-1yl)benzene as a yellow oil.

1. temperaturewarmed to ambient temperature
2. stirringThe resulting solution was stirred at 60° C. for 30 minutes
3. temperaturecooled to ambient temperature
4. concentrationconcentrated
5. customThe residue was triturated with 10% hexane in ethyl acetate
6. filtrationThe mixture was filtered through a silica gel pad
7. concentrationthe filtrate was concentrated