反应详情

A solution of 19 g (0.1 mol) dicyclohexylphosphine in 50 ml toluene was dropped into a suspension of 21 g (0.1 mol) PCl5 in 100 ml toluene. The reaction temperature was maintained at less than 30° C. After all had been dropped in, the whole was boiled for 1 hour under reflux. A slight precipitate was removed by means of a reverse frit and the reaction mixture was freed from all low boilers at 60° C. under 0.1 mbar. Yield: 23.3 g; 31P-NMR: δ P=126 ppm, (c-C6H11)2PCl, 96 mol %; δ P=54 ppm, (c-C6H11)2P(O)Cl, 3.7 mol %.

1. temperatureThe reaction temperature was maintained at less than 30° C
2. additionAfter all had been dropped in, the whole
3. temperatureunder reflux
4. customA slight precipitate was removed by means of a reverse frit
5. customwas freed from all low boilers at 60° C. under 0.1 mbar