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Potassium Iodide → 2-Bromo-9,9-didecyl-7-iodo-9H-fluorene

HRID 1268490
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HRID 1268490 반응식
[Br:1][C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6](=[CH:7][C:8]([I:15])=[CH:9][CH:10]=3)[CH2:5][C:4]=2[CH:3]=1.[I-].[K+].[OH-].[K+].Br[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30]>CS(C)=O>[Br:1][C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6](=[CH:7][C:8]([I:15])=[CH:9][CH:10]=3)[C:5]([CH2:13][CH2:14][CH2:2][CH2:3][CH2:4][CH2:12][CH2:11][CH2:10][CH2:9][CH3:8])([CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])[C:4]=2[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 81731-BromodecaneHCID 14797Potassium HydroxideHCID 142909822-Bromo-7-iodo-9H-fluorene

생성물 1

HCID 227234762-Bromo-9,9-didecyl-7-iodo-9H-fluorene수율 81%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

To a mechanically stirred mixture of 7-iodo-2-bromofluorene (from example 2; 41.34 g, 0.1114 mol), DMSO (100 mL), potassium iodide (1.7 g), and powdered potassium hydroxide (28 g) cooled in a cold water bath, 1-bromodecane (53 mL) was added dropwise, and the mixture was stirred for 24 hours. The oil that separated on dilution with water, was extracted with toluene. Toluene extract was washed with water, dried and concentrated. The residual oil was passed through a column of 300 g alumina. Elution with 900 mL hexanes gave the product as an oil, 65 g This was left in 200 mL of isopropanol, when the product solidified, 58.63 g (81% yield), m.p. 43-45° C. Mass Spec.: m/z 698 (M+ diiodo), 650,652 (M+).

후처리

  1. temperaturecooled in a cold water bath
  2. customThe oil that separated on dilution with water
  3. extractionwas extracted with toluene
  4. extractionToluene extract
  5. washwas washed with water
  6. customdried
  7. concentrationconcentrated
  8. washElution with 900 mL hexanes

출처 및 근거

ORD 기록
ord-178d6ef90add488a88928bd178ac3426
출처 데이터셋
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06555682B1

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