Triphenylphosphine → HCID 23031297, Verbindung

HRID 422942Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 422942
[I-:1].[NH:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[CH2:7][N+](C)(C)C.[C:12]1([P:18]([C:25]2C=CC=CC=2)[C:19]2C=CC=CC=2)C=CC=CC=1>C(#N)C>[I-:1].[NH:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[CH2:7][P+:18]([CH3:25])([CH3:19])[CH3:12]

Komponenten

4

Edukt 2

HCID 11776TriphenylphosphineHCID 139751381H-Pyrrole-2-methanaminium, N,N,N-trimethyl-, iodide (1:1)

Produkt 1

HCID 23031297HCID 23031297, VerbindungAusbeute 152,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

Subsequently, to a suspension of (pyrrol-2-yl)methyl trimethylammonium iodide (7.59 g, 28.52 mmol) obtained above in acetonitrile (60 ml) was added triphenylphosphine (8.98 g, 34.2 mmol) with stirring, and the resulting mixture was stirred at 80° C. for 6 hours. After cooling, the reaction mixture was concentrated to about one-half of its initial volume, to which was added ethyl acetate (100 ml). The crystals precipitated were collected by filtration, washed with ethyl acetate and dried in vacuo to afford (pyrrol-2-yl)methyl trimethylphosphonium iodide (12.33 g, yield: 92%).

Aufarbeitung

  1. stirringthe resulting mixture was stirred at 80° C. for 6 hours
  2. temperatureAfter cooling
  3. concentrationthe reaction mixture was concentrated to about one-half of its initial volume
  4. additionto which was added ethyl acetate (100 ml)
  5. customThe crystals precipitated
  6. filtrationwere collected by filtration
  7. washwashed with ethyl acetate
  8. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-763320038eca4cc085d3f690c3bd8d18
Quelldatensatz
uspto-grants-2012_01
Patentnummer
US08101650B2

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