Water → 3-Bromo-6-fluoro-2-methylbenzenamine

HRID 1771651ノート

反応式

HRID 1771651 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[C:4]([N+:9]([O-])=O)[C:3]=1[CH3:12].[NH4+].[Cl-].O>CCO.[Fe]>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[C:4]([NH2:9])[C:3]=1[CH3:12]

参加物

6

反応物 3

HCID 962WaterHCID 25517Ammonium ChlorideHCID 585404001-Bromo-4-fluoro-2-methyl-3-nitrobenzene

生成物 1

HCID 585401563-Bromo-6-fluoro-2-methylbenzenamine収率 77%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 702Ethanol溶媒

実験手順

To a solution of 1-bromo-4-fluoro-2-methyl-3-nitro-benzene (3 g, 12.82 mmol, 1.0 eq) in EtOH (60 mL) was added NH4Cl (30 mL), water (30 mL) and iron powder (2.87 g, 51.28 mmol, 4.0 eq). The reaction mixture was heated at reflux for 3h, then filtered through Celite. The filtrate was evaporated in vacuo and purified by column chromatography (EtOAc:petroleum ether, 0:1 to 1:10) to give the title compound as a yellow solid (2 g, 77%).

後処理

  1. temperatureThe reaction mixture was heated
  2. filtrationfiltered through Celite
  3. customThe filtrate was evaporated in vacuo
  4. custompurified by column chromatography (EtOAc:petroleum ether, 0:1 to 1:10)

出典と根拠

ORDレコード
ord-aeb1ebc553bf47c198af5002db95fe6c
出典データセット
uspto-grants-2016_02
特許番号
US09249085B2

反応ノート

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