Ammonium Chloride → 3,4-Difluoro-2-methoxyaniline

HRID 358885ノート

反応式

HRID 358885 の反応式
[Cl-].[NH4+].[F:3][C:4]1[C:5]([O:14][CH3:15])=[C:6]([N+:11]([O-])=O)[CH:7]=[CH:8][C:9]=1[F:10]>CO>[F:3][C:4]1[C:5]([O:14][CH3:15])=[C:6]([CH:7]=[CH:8][C:9]=1[F:10])[NH2:11]

参加物

4

反応物 2

HCID 25517Ammonium ChlorideHCID 27827542,3-Difluoro-6-nitroanisole

生成物 1

HCID 111374253,4-Difluoro-2-methoxyaniline収率 56.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

22.6 g (0.422 mole) of ammonium chloride and 38.2 g of reduced iron were added to a solution of 23.0 g (0.114 mole) of 3,4-difluoro-2-methoxy-1-nitrobenzene (VII) [prepared as described in step (a) above] in 1 liter of 80% aqueous methanol. The mixture was then heated under reflux for 4 hours, whilst stirring. At the end of this time, the reaction mixture was filtered, and the filtrate was concentrated by evaporation under reduced pressure. The residue was extracted with toluene. The toluene extract was washed with water, dried, and concentrated by evaporation under reduced pressure to give 10.2 g of 3,4-difluoro-2-methoxyaniline (VIII) as a reddish-brown oil [Step (B2)].

後処理

  1. temperatureThe mixture was then heated
  2. temperatureunder reflux for 4 hours
  3. filtrationAt the end of this time, the reaction mixture was filtered
  4. concentrationthe filtrate was concentrated by evaporation under reduced pressure
  5. extractionThe residue was extracted with toluene
  6. extractionThe toluene extract
  7. washwas washed with water
  8. customdried
  9. concentrationconcentrated by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-11eff042e4f847699b69513415f89e48
出典データセット
uspto-grants-1991_03
特許番号
US04997943

反応ノート

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