1,2-双(二氯磷基)-乙烷

反应条件: temp:-30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 250 ml of pentadecylmagnesium bromide (15% in tetrahydroluran (THF); 119 mmol) are initially charged in a 1|4-neck flask with internal thermometer, argon blanketing, metal/water condenser and stirrer, and cooled to −30° C. Subsequently, a solution of 5.5 g (23.8 mmol) of 1,2-bis(dichlorophosphino)-ethane in 100 ml of THF is added dropwise within 30 minutes, in the course of which a large amount of solids precipitates. The mixture is then warmed to room temperature within one hour and subsequently stirred at internal temperature 50° C. for a further 2 hours, which gives rise to a grayish-white suspension. This is admixed gradually, and while cooling with ice, with 95 ml of saturated and degassed NH4Cl solution to obtain a white suspension. Another 65 ml of degassed water are added thereto and the precipitate is filtered off with suction through a G2 frit under argon. The product is washed once with water and twice with 20 ml of THF, and dried under reduced pressure. This gives 22.2 g (93.5%) of the product in the form of a white powder. 31P NMR (CDCl3): −26.8 ppm (s); elemental analysis: calc. C 79.6%, H 13.8%, P 6.6%; exp. C 79.5%, H 14.0%, P 6.3%, Br 0.04%, Cl 0.06%, O<0.5%. precipitates The mixture is then warmed to room temperature within one hour which gives rise to a grayish-white suspension while cooling with ice, with 95 ml of saturated and degassed NH4Cl solution to obtain a white suspension the precipitate is filtered off with suction through a G2 frit under argon The product is washed once with water and twice with 20 ml of THF dried under reduced pressure