6-Bromo-1-nitronaphthalen-2-amine → 6-Bromonaphthalene-1,2-diamine

HRID 1751627ノート

反応式

HRID 1751627 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[C:8]([N+:12]([O-])=O)=[C:7]([NH2:15])[CH:6]=[CH:5]2>C(O)C.[Ni]>[Br:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([NH2:15])[C:8]=2[NH2:12])[CH:3]=1

参加物

4

反応物 1

HCID 218071856-Bromo-1-nitronaphthalen-2-amine

生成物 1

HCID 220970716-Bromonaphthalene-1,2-diamine収率 89.4%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

実験手順

To a mixture of 6-bromo-1-nitronaphthalen-2-amine (11.6 g, 43.4 mmol) in ethanol (430 mL) under argon was added Raney Nickel (˜5 g, NOTE: no effort was made to remove the water from the nickel). Hydrogen gas was bubbled through the reaction mixture for 2 minutes. The reaction was stirred under an atmosphere of hydrogen at room temperature. After 16 hours, the Raney Nickel was removed by filtration over Celite and rinsed with ethyl acetate. The filtrate was thoroughly concentrated to yield 6-bromonaphthalene-1,2-diamine (9.2 g, 88% yield).

後処理

  1. customto remove the water from the nickel)
  2. customHydrogen gas was bubbled through the reaction mixture for 2 minutes
  3. customthe Raney Nickel was removed by filtration over Celite
  4. washrinsed with ethyl acetate
  5. concentrationThe filtrate was thoroughly concentrated

出典と根拠

ORDレコード
ord-b11ee7811d074a498a47252296fd488e
出典データセット
uspto-grants-2015_10
特許番号
US09156823B2

反応ノート

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