反应详情

in ice bath, 3.14 g of malononitrile was added to the suspension of 2.45 g of sodium hydride (60% in oil solution) in 50 mL of ethylene glycol dimethyl ether, then the mixture was warmed to room temperature, stirred for 20 minutes and 3.68 g of 2,7-dibromo-9,9-dimethyl silafluorene and 0.54 g of PdCl2(PPh3)2 were added. The mixture was heated to 120° C. for 12 hours, cooled to 0° C., and saturated Br2/H2O solution was added. A water was added, and the resulting mixture was vacuum filtered, washed with water, dried, and column chromatographed to give the product. MALDI-TOF-MS (m/z): 336.4 (M+).

1. temperatureThe mixture was heated to 120° C. for 12 hours
2. temperaturecooled to 0° C.
3. filtrationfiltered
4. washwashed with water
5. customdried
6. customcolumn chromatographed
7. customto give the product