Iodine → 2-Bromo-7-iodo-9H-fluorene

HRID 31956

反応式

HRID 31956 の反応式
[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

参加物

7

反応物 4

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

生成物 1

HCID 142909822-Bromo-7-iodo-9H-fluorene収率 333.6%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒2 回

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9f1019e9f08e4c20928a76146f953959
出典データセット
uspto-grants-2008_09
特許番号
US07425654B2

関連ノート

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