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2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → (4-Methoxyphenyl)(2-phenylnaphthalen-1-yl)methanone

HRID 439328
ノート
印刷プレビュー

反応式

HRID 439328 の反応式
[C:1]1([C:7]2[CH2:8][CH2:9][C:10]3[C:15]([C:16]=2[C:17](=[O:26])[C:18]2[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=2)=[CH:14][CH:13]=[CH:12][CH:11]=3)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.ClC1C(=O)C(C#N)=C(C#N)C(=O)C=1Cl>O1CCOCC1>[CH3:25][O:24][C:21]1[CH:22]=[CH:23][C:18]([C:17]([C:16]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[CH:9]=[CH:8][C:7]=2[C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[O:26])=[CH:19][CH:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 67752,3-Dichloro-5,6-dicyano-1,4-benzoquinoneHCID 12835030(4-Methoxyphenyl)(2-phenyl-3,4-dihydronaphthalen-1-yl)methanone

生成物 1

HCID 22001239(4-Methoxyphenyl)(2-phenylnaphthalen-1-yl)methanone

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

The title product was prepared as described in U.S. Pat. No. 4,230,862. To 30 ml of dioxane were added 3-phenyl-4-(4-methoxybenzoyl)-1,2-dihydronaphthalene (1.90 g, 5.58 mmol), prepared as described in Example 3, supra, and 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (2.00 g, 8.81 mmol). The resulting mixture was heated to reflux and refluxed for twelve hours under a nitrogen atmosphere. The mixture was then cooled and evaporated to dryness. The residue was partitioned between ether and water. The organic fraction was washed 5N sodium hydroxide (5×20 ml), followed by a wash with brine. The mixture was then dried over magnesium sulfate and evaporated to give 1.9 grams of substantially pure 1-(4-methoxybenzoyl)-2-phenylnaphthalene.

後処理

  1. customprepared
  2. temperatureThe resulting mixture was heated
  3. temperatureto reflux
  4. temperaturerefluxed for twelve hours under a nitrogen atmosphere
  5. temperatureThe mixture was then cooled
  6. customevaporated to dryness
  7. customThe residue was partitioned between ether and water
  8. washThe organic fraction was washed 5N sodium hydroxide (5×20 ml)
  9. washa wash with brine
  10. dry with materialThe mixture was then dried over magnesium sulfate
  11. customevaporated

出典と根拠

ORDレコード
ord-43aab8513733468dacf91924cd098d84
出典データセット
uspto-grants-1996_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05514675

反応ノート

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