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Ethanol → 5-Bromo-o-toluidine

HRID 380040
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HRID 380040 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:11])=[C:6]([N+:8]([O-])=O)[CH:7]=1.[Cl-].[NH4+].C(O)C.[OH-].[Na+]>[Fe].O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:11])=[C:6]([CH:7]=1)[NH2:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 702EthanolHCID 14798Sodium HydroxideHCID 25517Ammonium ChlorideHCID 1235464-Bromo-2-nitrotoluene

생성물 1

HCID 27348055-Bromo-o-toluidine수율 102.2%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 962Water용매

실험 절차

A slurry of 5-bromo-2-methylnitrobenzene (3.00 g), iron powder (3.11 g), and ammonium chloride (2.97 g), in 3:1 ethanol : water (50 ml) was heated at reflux temperature for 1 hour. The mixture was poured into 10% aqueous sodium hydroxide and filtered through Celite®. The filtrate was then extracted with ethyl acetate, the extracts washed with brine, dried over magnesium sulfate, filtered and evaporated to afford the subtitle compound as an oil (2.64 g).

후처리

  1. temperatureat reflux temperature for 1 hour
  2. filtrationfiltered through Celite®
  3. extractionThe filtrate was then extracted with ethyl acetate
  4. washthe extracts washed with brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated

출처 및 근거

ORD 기록
ord-0afe2c257b8f4b8fba79f5c0eb0868fb
출처 데이터셋
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06300352B1

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