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Water → Methyl 4-(allylamino)-5-amino-3-fluoro-2-(2-fluoro-4-iodophenylamino)benzoate

HRID 1161785
ノート
印刷プレビュー

反応式

HRID 1161785 の反応式
[CH2:1]([NH:4][C:5]1[C:14]([N+:15]([O-])=O)=[CH:13][C:8]([C:9]([O:11][CH3:12])=[O:10])=[C:7]([NH:18][C:19]2[CH:24]=[CH:23][C:22]([I:25])=[CH:21][C:20]=2[F:26])[C:6]=1[F:27])[CH:2]=[CH2:3].[Cl-].[NH4+].O>CO.O1CCOCC1.[Fe]>[CH2:1]([NH:4][C:5]1[C:14]([NH2:15])=[CH:13][C:8]([C:9]([O:11][CH3:12])=[O:10])=[C:7]([NH:18][C:19]2[CH:24]=[CH:23][C:22]([I:25])=[CH:21][C:20]=2[F:26])[C:6]=1[F:27])[CH:2]=[CH2:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 962WaterHCID 25517Ammonium ChlorideHCID 58781109Methyl 4-(allylamino)-3-fluoro-2-(2-fluoro-4-iodophenylamino)-5-nitrobenzoate

生成物 1

HCID 58781154Methyl 4-(allylamino)-5-amino-3-fluoro-2-(2-fluoro-4-iodophenylamino)benzoate

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 887
Methanol
溶媒
HCID 312751,4-Dioxane溶媒

実験手順

A suspension of methyl 4-(allylamino)-3-fluoro-2-(2-fluoro-4-iodophenylamino)-5-nitrobenzoate and ammonium chloride (4.42 g, 79 mmoles) in a mixture of MeOH (20 ml) and dioxane (20 ml) is heated until it became a clear solution. Iron powder (4.42 g, 79 mmoles) is added and the resulting mixture is heated under reflux overnight. Water is added and the reaction mixture is filtered through celite. The solvent is removed under reduced pressure and the crude material is purified by flash chromatography to give the title compound.

後処理

  1. temperatureis heated until it
  2. temperaturethe resulting mixture is heated
  3. temperatureunder reflux overnight
  4. filtrationthe reaction mixture is filtered through celite
  5. customThe solvent is removed under reduced pressure
  6. customthe crude material is purified by flash chromatography

出典と根拠

ORDレコード
ord-3e944c5524a7433e927397f703ef09a2
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07820664B2

反応ノート

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