反应详情

温度

90 °C

To a solution of 1-bromo-4-iodo-2-methoxybenzene (L. A. Hasvold et al., US 2004/0254159) in MeCN (1.1 M) was added acrylic acid (1.24 eq.), TEA (2.5 eq.) and palladium acetate (0.03 eq). The reaction mixture was heated to 90° C. for 40 min, cooled to RT and poured into 1N HCl. After sting for 30 min, the solid was filtered, heated to reflux in EtOH (2.3 M), allowed to cool to RT and stirred overnight. The solid was filtered and washed with 1:1 EtOH:hexane to give the desired product 119. LRMS ESI+ (M+H)+ 257.0.

1. temperaturecooled to RT
2. filtrationthe solid was filtered
3. temperatureheated
4. temperatureto reflux in EtOH (2.3 M)
5. temperatureto cool to RT
6. filtrationThe solid was filtered
7. washwashed with 1:1 EtOH