反应详情

温度

0 °C

20 g (39 mmol) of tris(pentafluorophenyl)borane are suspended in 150 ml of heptane and, under reflux, a solution of 1.8 ml (97.5 mmol) of water in 40 ml of toluene is then added over a period of 30 minutes. The mixture is subsequently stirred for another five hours under reflux. The solution is subsequently cooled to 0° C. Over a period of 30 minutes, the product precipitates as a white solid. The product is isolated and washed three times with 50 ml each time of pentane and subsequently dried in an oil pump vacuum. This gives 11.5 g (80%) of colorless bis(pentafluorophenyl)hydroxyborane. The boroxin content is 10%. 1H-NMR(C6D6, 400 MHz): −133.1 (m, 4 F, o-B(C6F5)2), −147.9 (m, 2 F, p-B(C6F5)2), −161.1 (m, 4 F, m-B(C6F5)2) ppm.

1. temperatureunder reflux
2. temperatureunder reflux
3. waitOver a period of 30 minutes
4. customthe product precipitates as a white solid
5. customThe product is isolated
6. washwashed three times with 50 ml each time of pentane
7. customsubsequently dried in an oil pump vacuum