Hydrogen iodide → 2,6-Dibromoanthracene

HRID 506211ノート

反応式

HRID 506211 の反応式
[Br:1][C:2]1[CH:15]=[CH:14][C:13]2[C:12](=O)[C:11]3[C:6](=[CH:7][CH:8]=[C:9]([Br:17])[CH:10]=3)[C:5](=O)[C:4]=2[CH:3]=1.I.[PH2](O)=O>C(O)(=O)C>[Br:1][C:2]1[CH:15]=[CH:14][C:13]2[C:4](=[CH:5][C:6]3[C:11]([CH:12]=2)=[CH:10][C:9]([Br:17])=[CH:8][CH:7]=3)[CH:3]=1

参加物

5

反応物 3

HCID 24841Hydrogen iodideHCID 4124402Phosphinic AcidHCID 109594842,6-Dibromoanthraquinone

生成物 1

HCID 220589062,6-Dibromoanthracene

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Subsequently, a mixture of 2,6-dibromoanthraquinone (22.41 g, 61.23 mmol), acetic acid (250 mL), 56-58% hydriodic acid (100 mL), and 50% hypophosphorous acid (55 mL) was refluxed for 5 days. The mixture was then cooled to room temperature and poured into ice water (800 mL). Thereafter, the precipitate was filtered and washed with water and ethanol. The precipitate was then re-crystallized from toluene (620 mL) to give 14.49 g of pale yellow flake-like crystals of 2,6-dibromoanthracene (Compound 24).

後処理

  1. temperaturewas refluxed for 5 days
  2. filtrationThereafter, the precipitate was filtered
  3. washwashed with water and ethanol
  4. customThe precipitate was then re-crystallized from toluene (620 mL)

出典と根拠

ORDレコード
ord-9506387026d14b449bb4a3e21156d892
出典データセット
uspto-grants-2010_08
特許番号
US07781761B2

反応ノート

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