Iodine → 2-Iodo-9H-fluorene

HRID 746353

반응식

HRID 746353 반응식
[CH:1]1[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.II.[I:16](O)(=O)(=O)=O>C(O)(=O)C>[I:16][C:9]1[CH:8]=[CH:7][C:6]2[C:5]3[C:13](=[CH:1][CH:2]=[CH:3][CH:4]=3)[CH2:12][C:11]=2[CH:10]=1

참가 물질

5

반응물 3

HCID 807IodineHCID 6853FluoreneHCID 65185Metaperiodic acid

생성물 1

HCID 2240942-Iodo-9H-fluorene수율 644.4%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
80 °C

실험 절차

A 250 mL round-bottomed flask was charged with 20.0 g (120 mmol) fluorene, 16.0 g (60 mmol) iodine and 4.0 g (17 mmol) periodic acid. 150 mL (80%) acetic acid was added to the reaction mixture. The mixture was stirred under nitrogen at 80° C. for 4 hours. The mixture was then allowed to cool to ambient temperature. The solid residue was vacuum filtered, dissolved in toluene and then washed with 5% sodium hydrogen sulphite(to remove excess iodine). The toluene solution was concentrated under vacuo and then passed through a flash column using toluene as the eluent to give 32.0 g (91% yield) of the product (off white solid).

후처리

  1. temperatureto cool to ambient temperature
  2. filtrationfiltered
  3. dissolutiondissolved in toluene
  4. washwashed with 5% sodium hydrogen sulphite(to remove excess iodine)
  5. concentrationThe toluene solution was concentrated under vacuo

출처 및 근거

ORD 기록
ord-02d49db4e29a434d840bc7c12840f8c2
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07393599B2

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