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

HRID 358871노트

반응식

HRID 358871 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 27752772,4,5-Trifluoro-3-methoxyaniline수율 85.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4e78f93e281f4646b98739d707826e81
출처 데이터셋
uspto-grants-1991_03
특허 번호
US04997943

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