Methanol → 2-Amino-6-bromophenol

HRID 469804ノート

反応式

HRID 469804 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([Br:10])[C:5]=1[OH:11])([O-])=O.CO>C1COCC1.[Ni]>[NH2:1][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([Br:10])[C:5]=1[OH:11]

参加物

5

反応物 2

HCID 887MethanolHCID 135454532-Bromo-6-nitrophenol

生成物 1

HCID 155315062-Amino-6-bromophenol

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 8028Tetrahydrofuran溶媒

実験手順

5 g (22.9 mmol) 2-nitro-6-bromo-phenol (Fluka 67211) is hydrogenated in the presence of 0.1 g Ra—Ni (B113W EtOH, Degussa) in 100 ml of THF:MeOH=1:1. for 4 h. The reaction mixture is filtered (2 glass fiber filters used) and the filtrate is concentrated in vacuo. The residue is purified by chromatography (silicagel, hexane:EtOAc=2:1) to afford the title compound as a reddish oil which slowly solidifies.

後処理

  1. filtrationThe reaction mixture is filtered (2 glass fiber filters used)
  2. concentrationthe filtrate is concentrated in vacuo
  3. customThe residue is purified by chromatography (silicagel, hexane:EtOAc=2:1)

出典と根拠

ORDレコード
ord-991f4ad3cf6d4953aefaa3c986c6fd40
出典データセット
uspto-grants-2014_01
特許番号
US08629168B2

反応ノート

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