Ammonia → 3-Fluoro-2-nitroaniline

HRID 475224ノート

反応式

HRID 475224 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4](F)[C:3]=1[N+:9]([O-:11])=[O:10].[NH3:12]>CCO>[F:1][C:2]1[C:3]([N+:9]([O-:11])=[O:10])=[C:4]([NH2:12])[CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 222AmmoniaHCID 879221,3-Difluoro-2-nitrobenzene

生成物 1

HCID 27828343-Fluoro-2-nitroaniline収率 85%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
75 °C

実験手順

To a solution of 1,3-difluoro-2-nitro-benzene (30 g, 0.188 moles) in EtOH (300 mL) was added 25% aq. ammonia solution (300 mL) and the resulting mixture was heated to 75° C. for 16 h then cooled and concentrated in vacuo. The residue was dissolved in EtOAc, washed with water and brine solution, dried (Na2SO4), filtered and concentrated to afford 25 g (85%) of 3-fluoro-2-nitro-phenylamine (138) as a brown solid which was used without any further purification.

後処理

  1. temperaturethen cooled
  2. concentrationconcentrated in vacuo
  3. dissolutionThe residue was dissolved in EtOAc
  4. washwashed with water and brine solution
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-c5cc3d9576ed4eea843772b00f798f04
出典データセット
uspto-grants-2014_01
特許番号
US08637537B2

反応ノート

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