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2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → HCID 14722317、化合物

HRID 1031668
ノート
印刷プレビュー

反応式

HRID 1031668 の反応式
[CH3:1][O:2][CH:3]1[C:8](=[O:9])[C:7]2[CH:10]=[C:11]([O:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[C:12]([NH:14][S:15]([CH3:18])(=[O:17])=[O:16])=[CH:13][C:6]=2[O:5][CH2:4]1.ClC1C(=O)C(C#N)=C(C#N)C(=O)C=1Cl>O1CCOCC1>[CH3:1][O:2][C:3]1[C:8](=[O:9])[C:7]2[CH:10]=[C:11]([O:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[C:12]([NH:14][S:15]([CH3:18])(=[O:17])=[O:16])=[CH:13][C:6]=2[O:5][CH:4]=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 14722453HCID 14722453、化合物

生成物 1

HCID 14722317HCID 14722317、化合物収率 52.9%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

There were mixed 3.63 g of 2,3-dihydro-3-methoxy-7-methylsulfonylamino-6-phenoxy-4H-1-benzopyran4-one, 3.41 g of 2,3-dichloro-5,6-dicyano-1,4-benzoquinone and 150 ml of dioxane. The mixture was refluxed for 48 hours. The reaction mixture was cooled. The resulting precipitate was removed by filtration. The solvent was removed by distillation under reduced pressure. The residue was purified by a column chromatography (eluant: a 3 : 1 mixture of toluene and ethyl acetate) to obtain 1.91 g (yield: 52.9%) of 3-methoxy-7-methylsulfonylamino-6-phenoxy-4H-1-benzopyran-4-one [Compound No. 2].

後処理

  1. temperatureThe mixture was refluxed for 48 hours
  2. temperatureThe reaction mixture was cooled
  3. customThe resulting precipitate was removed by filtration
  4. customThe solvent was removed by distillation under reduced pressure
  5. customThe residue was purified by a column chromatography (eluant
  6. additiona 3 : 1 mixture of toluene and ethyl acetate)

出典と根拠

ORDレコード
ord-d28791e6ede9425e88289421b912d920
出典データセット
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04954518

反応ノート

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