2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → 2-Iodophenanthrene

HRID 68494ノート

反応式

HRID 68494 の反応式
[I:1][C:2]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[CH2:6][CH2:5][C:4]=2[CH:3]=1.ClC1C(=O)C(C#N)=C(C#N)C(=O)C=1Cl>O1CCOCC1>[I:1][C:2]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[CH:6]=[CH:5][C:4]=2[CH:3]=1

参加物

4

反応物 2

HCID 67752,3-Dichloro-5,6-dicyano-1,4-benzoquinoneHCID 576345402-Iodo-9,10-dihydrophenanthrene

生成物 1

HCID 123833792-Iodophenanthrene収率 78.9%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Under an argonatmosphere, 125 g of 2-iodo-9,10-dihydrophenanthrene, 98 g of 2,3-dichloro-5,6-dicyano-p-benzoquinone, and 1.2 L of 1,4-dioxane were added, and then the mixture was stirred for 24 hours under heating reflux. After having been cooled to room temperature, the reaction solution was concentrated. The residue was purified by silica gel column chromatography, and was then washed with methanol. Thus, 98 g of a white crystal were obtained (in 68% yield).

後処理

  1. temperatureunder heating
  2. temperaturereflux
  3. concentrationthe reaction solution was concentrated
  4. customThe residue was purified by silica gel column chromatography
  5. washwas then washed with methanol

出典と根拠

ORDレコード
ord-245af911a1244422b6976035c608e6bb
出典データセット
uspto-grants-2014_09
特許番号
US08822041B2

反応ノート

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