Triphenylphosphine → HCID 21293727, Verbindung

HRID 622118

Reaktionsgleichung

Reaktionsgleichung von HRID 622118
[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH:12]=[C:13]([CH3:15])[CH3:14].[C:16]1([P:22]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>C(#N)C>[Br-:1].[CH3:14][C:13]([CH3:15])=[CH:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][P+:22]([C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1)([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1

Komponenten

4

Edukt 2

HCID 11776TriphenylphosphineHCID 212937251-Bromo-12-methyl-11-tridecene

Produkt 1

HCID 21293727HCID 21293727, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

1-Bromo-12-methyl-11-tridecene (4.4 g, 16 mmoles) and triphenylphosphine (4.65 g, 17 mmoles) dissolved in acetonitrile (80 ml) were heated to reflux for 4 days, cooled and concentrated in vacuo. The residue was chromatographed on silica gel eluted with chloroform and then with methanol-chloroform (2:3). Fractions containing the product were concentrated in vacuo, triturated with ether, filtered and dried in vacuo to afford the desired phosphonium salt.

Aufarbeitung

  1. temperaturewere heated
  2. temperatureto reflux for 4 days
  3. temperaturecooled
  4. concentrationconcentrated in vacuo
  5. customThe residue was chromatographed on silica gel
  6. washeluted with chloroform
  7. additionFractions containing the product
  8. concentrationwere concentrated in vacuo
  9. customtriturated with ether
  10. filtrationfiltered
  11. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-d27479dc65674ab59cc4d7907eef6fa5
Quelldatensatz
uspto-grants-1988_09
Patentnummer
US04769386

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