Cesium carbonate → HCID 86617330, Verbindung

HRID 1960211Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1960211
I[C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]([O:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:10]=[CH:11][O:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Cs+].[Cs+].[C:32](P(C(C)(C)C)C(C)(C)C)(C)(C)[CH3:33].C([Sn](CCCC)(CCCC)C=C)CCC>O1CCOCC1>[CH:32]([C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]([O:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:10]=[CH:11][O:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[CH:4][CH:3]=1)=[CH2:33]

Komponenten

6

Edukt 4

HCID 10796Cesium carbonateHCID 81998TributylvinyltinHCID 83681Tris(1,1-dimethylethyl)phosphineHCID 86617331HCID 86617331, Verbindung

Produkt 1

HCID 86617330HCID 86617330, VerbindungAusbeute 75 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

Phenyl N-(4-iodophenyl)-3-(phenoxy)acrylimidate (0.50 g), bis(benzylideneacetone)palladium (0) (0.023 g) and cesium carbonate (0.82 g) were suspended to dioxane (15 ml). Tri-t-butylphosphine (10 wt % in hexane: 0.24 g) and tributyl (vinyl) tin (0.44 g) were added thereto and it was stirred for four hours at room temperature and 60° C. for five hours. The unsolved matter was filtered off, and the filtrate was concentrated under reduced pressure. The residue was separated and purified by silica gel column chromatography (hexane:ethyl acetate=30:1) to obtain phenyl N-(4-vinylphenyl)-3-(phenoxy)acrylimidate (0.29 g) as yellow oil.

Aufarbeitung

  1. filtrationThe unsolved matter was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe residue was separated
  4. custompurified by silica gel column chromatography (hexane:ethyl acetate=30:1)

Quellen und Nachweise

ORD-Eintrag
ord-4f4b74eb225c406a80bdc46e7110eba4
Quelldatensatz
uspto-grants-2013_04
Patentnummer
US08410316B2

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