反应详情

温度

100 °C

A mixture of 50.0 g (289 mmol) of 4-bromofluorobenzene, 43.3 g (318 mmol) of isobutyl methanephosphonite, 43.8 ml (318 mmol) of triethylamine, 1.64 g (0.29 mmol,1 mol %) of bis(dibenzylideneacetone)-palladium and 1.50 g (0.58 mmol, 2 mol %) of triphenylphosphine was heated for 20 hours at 100° C. under an inert gas atmosphere. At 23° C., the solution was filtered off from the ammonium salt formed and the filtrate was evaporated under reduced pressure. Fractional distillation under reduced pressure gave 54.60 g (83% of theory) of isobutyl 4-fluorophenylmethylphosphinate having a boiling point of 83° C./0.08 mbar.

1. filtrationAt 23° C., the solution was filtered off from the ammonium salt
2. customformed
3. customthe filtrate was evaporated under reduced pressure
4. distillationFractional distillation under reduced pressure