반응 #60234

반응 방정식

2-bromofluorene

orthoperiodic acid

sulfuric acid

iodine

→

yellow crystal

2-bromo-7-iodofluorene

용매

water

water

acetic acid

반응 조건

후처리

1. 1
   workup.ADDITIONCharged
2. 2
   기타was elevated up to 90° C.
3. 3
   온도the mixture was heated for 3 hours
4. 4
   workup.STIRRINGwhile stirring
5. 5
   workup.WAITThe reaction solution was left
6. 6
   온도cooling down to room temperature
7. 7
   기타The precipitate formed
8. 8
   여과was filtered
9. 9
   세척washed with ethanol and water
10. 10
    기타The solid matter thus obtained
11. 11
    기타was recrystallized from ethanol

실험 절차

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.

출처