Phosphorus pentachloride → Dibutylchlorophosphine

HRID 580365노트

반응식

HRID 580365 반응식
[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]

참가 물질

4

반응물 2

HCID 24819Phosphorus pentachlorideHCID 74419Phosphine, dibutyl-

생성물 1

HCID 305896Dibutylchlorophosphine수율 55.9%

시약·촉매·용매 1

HCID 24387Phosphorus trichloride용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-59cbf71311cf4f3cad9c3b4af5d6e4d9
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04752648

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