Iodine → 2-Bromo-7-iodo-9H-fluorene

HRID 31956

반응식

HRID 31956 반응식
[Br:1][C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[CH2:5][C:4]=2[CH:3]=1.II.[I:17](O)(O)(O)(O)(O)=O.S(=O)(=O)(O)O>O.C(O)(=O)C>[Br:1][C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6](=[CH:7][C:8]([I:17])=[CH:9][CH:10]=3)[CH2:5][C:4]=2[CH:3]=1

참가 물질

7

반응물 4

HCID 807IodineHCID 1118Sulfuric AcidHCID 143362-Bromo-9H-fluoreneHCID 25289Orthoperiodic acid

생성물 1

HCID 142909822-Bromo-7-iodo-9H-fluorene수율 333.6%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매2회

반응 조건

온도
60 °C

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.

후처리

  1. additionCharged
  2. customwas elevated up to 90° C.
  3. temperaturethe mixture was heated for 3 hours
  4. stirringwhile stirring
  5. waitThe reaction solution was left
  6. temperaturecooling down to room temperature
  7. customThe precipitate formed
  8. filtrationwas filtered
  9. washwashed with ethanol and water
  10. customThe solid matter thus obtained
  11. customwas recrystallized from ethanol

출처 및 근거

ORD 기록
ord-9f1019e9f08e4c20928a76146f953959
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07425654B2

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