Water → 3-Bromo-6-fluoro-2-methylbenzenamine

HRID 1771651노트

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HRID 1771651 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[C:4]([N+:9]([O-])=O)[C:3]=1[CH3:12].[NH4+].[Cl-].O>CCO.[Fe]>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[C:4]([NH2:9])[C:3]=1[CH3:12]

참가 물질

6

반응물 3

HCID 962WaterHCID 25517Ammonium ChlorideHCID 585404001-Bromo-4-fluoro-2-methyl-3-nitrobenzene

생성물 1

HCID 585401563-Bromo-6-fluoro-2-methylbenzenamine수율 77%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 702Ethanol용매

실험 절차

To a solution of 1-bromo-4-fluoro-2-methyl-3-nitro-benzene (3 g, 12.82 mmol, 1.0 eq) in EtOH (60 mL) was added NH4Cl (30 mL), water (30 mL) and iron powder (2.87 g, 51.28 mmol, 4.0 eq). The reaction mixture was heated at reflux for 3h, then filtered through Celite. The filtrate was evaporated in vacuo and purified by column chromatography (EtOAc:petroleum ether, 0:1 to 1:10) to give the title compound as a yellow solid (2 g, 77%).

후처리

  1. temperatureThe reaction mixture was heated
  2. filtrationfiltered through Celite
  3. customThe filtrate was evaporated in vacuo
  4. custompurified by column chromatography (EtOAc:petroleum ether, 0:1 to 1:10)

출처 및 근거

ORD 기록
ord-aeb1ebc553bf47c198af5002db95fe6c
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09249085B2

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