Reaktion #155676

Reaktionsgleichung

2-iodo-9,10-dihydrophenanthrene

2,3-dichloro-5,6-dicyano-p-benzoquinone

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white crystal

Ausbeute 78.9%

2-iodophenanthrene

Ausbeute 78.9%

Lösungsmittel

1,4-dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder heating
2. 2
   Temperaturreflux
3. 3
   Einengenthe reaction solution was concentrated
4. 4
   SonstigeThe residue was purified by silica gel column chromatography
5. 5
   Waschenwas then washed with methanol

Vorschrift

Under an argonatmosphere, 125 g of 2-iodo-9,10-dihydrophenanthrene, 98 g of 2,3-dichloro-5,6-dicyano-p-benzoquinone, and 1.2 L of 1,4-dioxane were added, and then the mixture was stirred for 24 hours under heating reflux. After having been cooled to room temperature, the reaction solution was concentrated. The residue was purified by silica gel column chromatography, and was then washed with methanol. Thus, 98 g of a white crystal were obtained (in 68% yield).

Quelle