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Triphenylphosphine → Phosphonium, nonyltriphenyl-, bromide (1:1)

HRID 365039
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HRID 365039 반응식
[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].[C:11]1([P:17]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>C(Cl)Cl>[Br-:1].[CH2:2]([P+:17]([C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1)([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)[C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10]
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참가 물질

4

반응물 2

HCID 11776TriphenylphosphineHCID 127421-Bromononane

생성물 1

HCID 2724864Phosphonium, nonyltriphenyl-, bromide (1:1)

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
100 °C

실험 절차

A magnetically stirred suspension of 1-bromononane (Aldrich, 40 g, 0.1931M) and triphenylphosphine (101.3 g, 0.3862 mole) was heated at 100° C. (oil bath) for 2 hours. The resulting homogeneous solution was then cooled and triturated with ether (8X) to remove most of the unreacted triphenylphosphine. A viscous gum was obtained which was dissolved in CH2Cl2 and concentrated in vacuo to give the title phosphonium salt as a light yellow, extremely hygroscopic foam weighing 85 g (80.1%). TLC, neat CH2Cl2, Rf =0.78, PMA.

후처리

  1. temperatureThe resulting homogeneous solution was then cooled
  2. customtriturated with ether (8X)
  3. customto remove most of the unreacted triphenylphosphine
  4. customA viscous gum was obtained which
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-271c3869a1e246b8ab90e30c700e5837
출처 데이터셋
uspto-grants-1986_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04607053

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