反应详情

温度

80 °C

A mixture of 2 g 5-bromo-1,3-difluoro-2-methoxy-benzene, 1.76 g ethynyl-trimethyl-silane, 629 mg bis(triphenylphosphine)palladium(II) dichloride, 3.1 ml diisopropylethylamine, and 85 mg copper iodide in 20 ml acetonitrile was degassed then heated at 80° C. for 2 hours. The mixture was diluted with dichloromethane and filtered through a plug of silica, washed with dilute ammonia and brine then dried over sodium sulphate, filtered and concentrated in vacuo. Purification over silica afforded 1.71 g (3,5-difluoro-4-methoxy-phenylethynyl)-trimethyl-silane.

1. customwas degassed
2. additionThe mixture was diluted with dichloromethane
3. filtrationfiltered through a plug of silica
4. washwashed with dilute ammonia and brine
5. dry with materialthen dried over sodium sulphate
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customPurification over silica