1,8-Diazabicyclo(5.4.0)undec-7-ene → HCID 86646305, Verbindung

HRID 1876280Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1876280
C1(P([N:15]=[N+:16]=[N-:17])(C2C=CC=CC=2)=O)C=CC=CC=1.N12CCCN=C1CCCCC2.[Cl:29][C:30]1[CH:39]=[C:38]2[C:33]([CH:34]=[CH:35][CH:36]=[C:37]2[CH2:40]O)=[CH:32][CH:31]=1>C1(C)C=CC=CC=1>[N:15]([CH2:40][C:37]1[C:38]2[C:33](=[CH:32][CH:31]=[C:30]([Cl:29])[CH:39]=2)[CH:34]=[CH:35][CH:36]=1)=[N+:16]=[N-:17]

Komponenten

5

Edukt 3

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 199401P,P-Diphenylphosphinic azideHCID 68697042HCID 68697042, Verbindung

Produkt 1

HCID 86646305HCID 86646305, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

1.52 ml of Diphenylphosphoryl azide and 1.10 ml of 1,8-diazabicyclo[5.4.0]undec-7-ene are added to 1.3 g of (7-Chloro-naphthalen-1-yl)-methanol in 18 ml of toluene. The mixture obtained is stirred at rt for 1 hour, washed with brine, the organic phase is dried and solvent is evaporated. The residue obtained is purified by flash chromatography on silica gel (eluent: cyclohexane/EtOAc 99/1) to yield the title compound.

Aufarbeitung

  1. customThe mixture obtained
  2. washwashed with brine
  3. customthe organic phase is dried
  4. customsolvent is evaporated
  5. customThe residue obtained
  6. customis purified by flash chromatography on silica gel (eluent: cyclohexane/EtOAc 99/1)

Quellen und Nachweise

ORD-Eintrag
ord-b045cfdf220a43718220c8c78611f6a2
Quelldatensatz
uspto-grants-2012_11
Patentnummer
US08309596B2

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