Toluene → HCID 178435532, Verbindung

HRID 1368558Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1368558
BrC1C=C2C(=CC=1)[CH:8]=[C:7]([C:12]([C:17]1[N:18]=[CH:19][N:20](C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[CH:21]=1)([OH:16])[CH:13]([CH3:15])[CH3:14])[CH:6]=[CH:5]2.[CH2:41](C([Sn])=C(CCCC)CCCC)CCC.[C:56]1([CH3:62])[CH:61]=[CH:60][CH:59]=[CH:58][CH:57]=1>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH2:62]([C:56]1[CH:61]=[C:60]2[C:59](=[CH:58][CH:57]=1)[CH:8]=[C:7]([C:12]([C:17]1[N:18]=[CH:19][NH:20][CH:21]=1)([OH:16])[CH:13]([CH3:15])[CH3:14])[CH:6]=[CH:5]2)[CH3:41]

Komponenten

5

Edukt 3

HCID 1140TolueneHCID 22018349HCID 22018349, VerbindungHCID 53438229Tri(butyl)vinyltin

Produkt 1

HCID 178435532HCID 178435532, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 178418397HCID 178418397, VerbindungKatalysator

Versuchsvorschrift

A solution of 1-(6-bromonaphthalen-2-yl)-2-methyl-1-(1-trityl-1H-imidazol-4-yl)-1-propanol (2.0 g), tetrakis(triphenylphosphine)palladium (116 mg) and tributylvinyltin (1.40 ml) in toluene (30 ml) was refluxed under argon atmosphere for 80 min. The solvent was distilled off and the residue was purified by column chromatography (eluent, hexane:THF=2:1),then crystallized from isopropyl ether-hexane (1:1) to give the titled compound (1.47 g) as a colorless powder.

Aufarbeitung

  1. distillationThe solvent was distilled off
  2. customthe residue was purified by column chromatography (eluent, hexane
  3. customTHF=2:1),then crystallized from isopropyl ether-hexane (1:1)

Quellen und Nachweise

ORD-Eintrag
ord-9f165b7ede0e476da5876cebb700d18a
Quelldatensatz
uspto-grants-2003_06
Patentnummer
US06573289B1

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