Reaktion #74974

Reaktionsgleichung

Hexachlorocyclopentadiene

1,4-naphthoquinone

→

1,2,3,4,11,11-hexachloro-1,4,4a,9a-tetrahydro-1,4-methanoanthracene-9,10-dione

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated
2. 2
   Temperaturto reflux temperature
3. 3
   Temperaturmaintained at this temperature for 4 hours
4. 4
   Extraktionextracting the excess hexachlorocyclopentadiene with Skelly "B" solvent
5. 5
   SonstigeThis crude brown solid was recrystallized repeatedly from benzene/Skelly "B" mix-solvent (70/30)
6. 6
   Sonstigeto yield white crystals, m.p. 116°-118° C.

Vorschrift

Hexachlorocyclopentadiene (60 g.), 1,4-naphthoquinone (31.6 g.), and 30 ml. of toluene were mixed, heated to reflux temperature, and maintained at this temperature for 4 hours. After cooling to room temperature and extracting the excess hexachlorocyclopentadiene with Skelly "B" solvent, the mixture solidified slowly. This crude brown solid was recrystallized repeatedly from benzene/Skelly "B" mix-solvent (70/30) to yield white crystals, m.p. 116°-118° C.

Quelle