Hydrochloric Acid → 3-Bromo-5-fluoro-2-methylaniline

HRID 1692740노트

반응식

HRID 1692740 반응식
[Br:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[C:4]([N+:9]([O-])=O)[C:3]=1[CH3:12].Cl>CO.C(Cl)Cl.[Fe]>[Br:1][C:2]1[C:3]([CH3:12])=[C:4]([NH2:9])[CH:5]=[C:6]([F:8])[CH:7]=1

참가 물질

6

반응물 2

HCID 313Hydrochloric AcidHCID 27733851-Bromo-5-fluoro-2-methyl-3-nitrobenzene

생성물 1

HCID 27376413-Bromo-5-fluoro-2-methylaniline수율 28.1%

시약·촉매·용매 3

HCID 23925Iron촉매HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

To a solution of crude 1-bromo-5-fluoro-2-methyl-3-nitro-benzene (5.96 g) in MeOH (90 mL) was added concentrated hydrochloric acid (11.7 mL) and iron (6.1 g) and the reaction mixture was heated to reflux. After 16 h, the mixture was cooled, diluted with DCM, washed with sodium carbonate solution, dried (MgSO4) and the solvent removed in vacuo. The residue was purified using flash chromatography to yield 3-bromo-5-fluoro-2-methyl-phenylamine (1.46 g).

후처리

  1. temperaturethe reaction mixture was heated to reflux
  2. temperaturethe mixture was cooled
  3. washwashed with sodium carbonate solution
  4. dry with materialdried (MgSO4)
  5. customthe solvent removed in vacuo
  6. customThe residue was purified

출처 및 근거

ORD 기록
ord-fc32c4fad49a4e9c8c7a4af179fd9a6c
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08158626B2

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