dibutyl(chloro)phosphane

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 148 g (1 mol) di-n-butylphosphine was dropped at a maximum reaction temperature of 30° C. into a suspension of 232 g (1.1 mol) PCl5 in 500 ml toluene. HCl and PCl3 formed during the reaction were removed under a vacuum of 130 mbar and condensed in a cooling trap. After the reaction was complete, the reaction mixture was found to comprise two liquid phases. The upper phase contained PCl3 in toluene. The bulk quantity of chlorophosphine was in the lower phase (31P-NMR). It was worked up distillatively and 101 g product was obtained (55% of the theoretical). bp 92° C./16 mbar. formed during the reaction were removed under a vacuum of 130 mbar and condensed in a cooling trap

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: di-1-Adamantyl-n-butylphosphine was procured from Strem, 77672 Kehl, Germany; 1-adamantyldi-n-butylphosphine was prepared from adamantylmagnesium bromide (J. Org. Chem. 47 1982 4120-4128) and chlorodi-n-butylphosphine (from Aldrich, 82018 Taufkirchen, Germany).

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: di-1-Adamantyl-n-butylphosphine was procured from Strem, 77672 Kehl, Germany; 1-adamantyldi-n-butylphosphine was prepared from adamantylmagnesium bromide (J. Org. Chem. 47 1982 4120-4128) and chlorodi-n-butylphosphine (from Aldrich, 82018 Taufkirchen, Germany).

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: di-1-Adamantyl-n-butylphosphine was procured from Strem, 77672 Kehl, Germany; 1-adamantyldi-n-butylphosphine was prepared from adamantylmagnesium bromide (J. Org. Chem. 47 1982 4120-4128) and chlorodi-n-butylphosphine (from Aldrich, 82018 Taufkirchen, Germany).

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 148 g (1 mol) di-n-butylphosphine was dropped at a maximum reaction temperature of 30° C. into a suspension of 232 g (1.1 mol) PCl5 in 500 ml toluene. HCl and PCl3 formed during the reaction were removed under a vacuum of 130 mbar and condensed in a cooling trap. After the reaction was complete, the reaction mixture was found to comprise two liquid phases. The upper phase contained PCl3 in toluene. The bulk quantity of chlorophosphine was in the lower phase (31P-NMR). It was worked up distillatively and 101 g product was obtained (55% of the theoretical). bp 92° C./16 mbar. formed during the reaction were removed under a vacuum of 130 mbar and condensed in a cooling trap