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Ammonium Chloride → 3-Bromobenzene-1,2-diamine

HRID 1399887
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HRID 1399887 반응식
[Br:1][C:2]1[C:3]([N+:9]([O-])=O)=[C:4]([CH:6]=[CH:7][CH:8]=1)[NH2:5].[NH4+].[Cl-]>CCO.O.[Fe]>[Br:1][C:2]1[CH:8]=[CH:7][CH:6]=[C:4]([NH2:5])[C:3]=1[NH2:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 25517Ammonium ChlorideHCID 218520723-Bromo-2-nitroaniline

생성물 1

HCID 124898393-Bromobenzene-1,2-diamine수율 98.8%

시약·촉매·용매 3

HCID 23925Iron촉매HCID 702Ethanol용매HCID 962Water용매

실험 절차

A mixture of 3-bromo-2-nitroaniline (2 g, 9.2 mmol), Fe powder (1.54 g, 27.6 mmol) and NH4Cl (4.8 g, 52 mmol) in EtOH and H2O was stirred under reflux for 1 h. The mixture was cooled to room temperature and filtered. The filtrate was diluted water extracted with ethyl acetate and the combined organic layers were dried and concentrated in vacuum to give the crude desired product (1.7 g, Yield 85%). This crude was used in the next step without further purification.

후처리

  1. temperatureunder reflux for 1 h
  2. filtrationfiltered
  3. extractionextracted with ethyl acetate
  4. customthe combined organic layers were dried
  5. concentrationconcentrated in vacuum

출처 및 근거

ORD 기록
ord-83fe1d2195394557acef6467367e23f8
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08906900B2

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