Reaktion #60234

Reaktionsgleichung

2-bromofluorene

orthoperiodic acid

sulfuric acid

iodine

→

yellow crystal

2-bromo-7-iodofluorene

Lösungsmittel

water

water

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONCharged
2. 2
   Sonstigewas elevated up to 90° C.
3. 3
   Temperaturthe mixture was heated for 3 hours
4. 4
   workup.STIRRINGwhile stirring
5. 5
   workup.WAITThe reaction solution was left
6. 6
   Temperaturcooling down to room temperature
7. 7
   SonstigeThe precipitate formed
8. 8
   Filtrationwas filtered
9. 9
   Waschenwashed with ethanol and water
10. 10
    SonstigeThe solid matter thus obtained
11. 11
    Sonstigewas recrystallized from ethanol

Vorschrift

Charged were 2-bromofluorene 25.0 g, iodine 11.5 g, orthoperiodic acid 4.88 g, acetic acid 150 ml, conc. sulfuric acid 3 ml and water 10 ml, and the mixture was heated at 60° C. for 30 minutes while stirring. Further, the temperature was elevated up to 90° C., and the mixture was heated for 3 hours while stirring. The reaction solution was left cooling down to room temperature and poured into 500 ml of water. The precipitate formed was filtered and washed with ethanol and water. The solid matter thus obtained was recrystallized from ethanol to obtain 26.5 g of yellow crystal of 2-bromo-7-iodofluorene.

Quelle