Phosphorus pentachloride → Dibutylchlorophosphine

HRID 580365ノート

反応式

HRID 580365 の反応式
[CH2:1]([PH:5][CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4].P(Cl)(Cl)(Cl)(Cl)[Cl:11]>P(Cl)(Cl)Cl>[CH2:1]([P:5]([CH2:6][CH2:7][CH2:8][CH3:9])[Cl:11])[CH2:2][CH2:3][CH3:4]

参加物

4

反応物 2

HCID 24819Phosphorus pentachlorideHCID 74419Phosphine, dibutyl-

生成物 1

HCID 305896Dibutylchlorophosphine収率 55.9%

試薬・触媒・溶媒 1

HCID 24387Phosphorus trichloride溶媒

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.

後処理

  1. customformed during the reaction
  2. customwere removed under a vacuum of 130 mbar and condensed in a cooling trap

出典と根拠

ORDレコード
ord-59cbf71311cf4f3cad9c3b4af5d6e4d9
出典データセット
uspto-grants-1988_06
特許番号
US04752648

反応ノート

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