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

HRID 1443630노트

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HRID 1443630 반응식
[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

참가 물질

4

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온도
40 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d6b16224bb4d42a892394ffb8c76c5bd
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07662581B1

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