Hydrazine hydrate (1:1) → 2,4,5-Trifluoro-3-methoxyaniline

HRID 358871ノート

反応式

HRID 358871 の反応式
O.NN.[CH3:4][O:5][C:6]1[C:7]([F:25])=[C:8]([N:14]2C(=O)C3=CC=CC=C3C2=O)[CH:9]=[C:10]([F:13])[C:11]=1[F:12]>C(O)C>[CH3:4][O:5][C:6]1[C:7]([F:25])=[C:8]([CH:9]=[C:10]([F:13])[C:11]=1[F:12])[NH2:14]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 20067133N-(3-Methoxy-2,4,5-trifluorophenyl)-phthalimide

生成物 1

HCID 27752772,4,5-Trifluoro-3-methoxyaniline収率 85.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

1.1 g (0.02 mole) of hydrazine hydrate was added to a suspension of 2.15 g (0.007 mole) of N-(3-methoxy-2,4,5-trifluorophenyl)phthalimide (XXXVI) [prepared as described in Step (F3) above] in 30 ml of ethanol, and the mixture was heated under reflux with stirring for 2 hours. The reaction mixture was cooled to room temperature and then filtered. The filtrate was concentrated by evaporation under reduced pressure, and the residue was dissolved in toluene. The resulting solution was washed with water and dried, and the solvent was then removed by evaporation under reduced pressure to afford 1.06 g of 3-methoxy-2,4,5-trifluoroaniline (XXIII) as pale brown needles.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated by evaporation under reduced pressure
  5. dissolutionthe residue was dissolved in toluene
  6. washThe resulting solution was washed with water
  7. customdried
  8. customthe solvent was then removed by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-4e78f93e281f4646b98739d707826e81
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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