N-benzyl-4-bromo-2-nitroaniline → 2-Benzylamino-5-bromoaniline

HRID 1443630ノート

反応式

HRID 1443630 の反応式
[CH2:1]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([Br:15])=[CH:11][C:10]=1[N+:16]([O-])=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>C(O)(=O)C.[Fe]>[CH2:1]([NH:8][C:9]1[C:10]([NH2:16])=[CH:11][C:12]([Br:15])=[CH:13][CH:14]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 1

HCID 24902949N-benzyl-4-bromo-2-nitroaniline

生成物 1

HCID 289029062-Benzylamino-5-bromoaniline

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 176Acetic Acid溶媒

反応条件

温度
40 °C

実験手順

To a solution of benzyl-(4-bromo-2-nitro-phenyl)-amine (276 mg, 0.9 mmol) in 3 ml acetic acid, was added iron (70 mg, 1.2 mmol). The reaction mixture was heated to 40° C. under argon for 2 hours. The mixture was cooled to ambient temperature and filtered through celite and the filtrate was concentrated. The resulting solid was dissolved in ethyl acetate. The organic layer was washed with saturated NaHCO3, dried over MgSO4, filtered and the filtrate was concentrated in vacuo to yield crude product that was used in Example 6c.

後処理

  1. temperatureThe mixture was cooled to ambient temperature
  2. filtrationfiltered through celite
  3. concentrationthe filtrate was concentrated
  4. dissolutionThe resulting solid was dissolved in ethyl acetate
  5. washThe organic layer was washed with saturated NaHCO3
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationthe filtrate was concentrated in vacuo
  9. customto yield crude product that

出典と根拠

ORDレコード
ord-d6b16224bb4d42a892394ffb8c76c5bd
出典データセット
uspto-grants-2010_02
特許番号
US07662581B1

反応ノート

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