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

HRID 1581871
ノート
印刷プレビュー

反応式

HRID 1581871 の反応式
[Br:1][C:2]1[CH:14]=[C:13]2[C:5]([C:6]3[CH:7]=[CH:8][C:9](C=O)=[CH:10][C:11]=3[C:12]2([CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH3:34])[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])=[CH:4][CH:3]=1.[I-:37].[K+].[OH-].[K+].BrCCCCCCCCCC>CS(C)=O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6]3[C:11](=[CH:10][C:9]([I:37])=[CH:8][CH:7]=3)[C:12]([CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH3:34])([CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])[C:13]=2[CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 81731-BromodecaneHCID 14797Potassium HydroxideHCID 22723474HCID 22723474、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

To a mechanically stirred mixture of 7-iodo-2-bromofluorene (example 2; 41.34 g, 0.1 114 mol), DMSO (100 mL), potassium iodide (1.79 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 isopropanola when the product solidified, 58.63 g (81% yield), m.p. 43-45° C. Mass Spec. (m/z): 698 (M+ diiodo), 650, 652 (M+).

後処理

  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

出典と根拠

ORDレコード
ord-4c6b8c88f8ca470aaf71c36641270ff0
出典データセット
uspto-grants-2004_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06730793B1

反応ノート

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