Sulfuric Acid → 1-bromo-3-ethyl-5-nitroBenzene

HRID 1452050

반응식

HRID 1452050 반응식
[CH2:1]([C:3]1[CH:9]=[C:8]([Br:10])[C:6](N)=[C:5]([N+:11]([O-:13])=[O:12])[CH:4]=1)[CH3:2].S(=O)(=O)(O)O.N([O-])=O.[Na+]>C(O)C>[Br:10][C:8]1[CH:6]=[C:5]([N+:11]([O-:13])=[O:12])[CH:4]=[C:3]([CH2:1][CH3:2])[CH:9]=1

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 199734682-Bromo-4-ethyl-6-nitroanilineHCID 23668193Sodium Nitrite

생성물 1

HCID 189298701-bromo-3-ethyl-5-nitroBenzene

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Dissolve 4-ethyl-2-nitro-6-bromoaniline (6.62g, 27mmol) in ethanol (40mL). Add, by dropwise addition, concentrated sulfuric acid (5mL) and heat at reflux, adding sodium nitrite (4.55g, mmol) in small portions over 25 minutes. Stir at room temperature for several hours, pour onto ice and extract into ethyl acetate. Wash with water (3×) and brine (3×). Dry (MgSO4) and evaporate the solvent in vacuo and purify by silica gel chromatography to give 3-bromo-5-ethylnitrobenzene.

후처리

  1. temperatureheat
  2. temperatureat reflux
  3. additionpour onto ice
  4. extractionextract into ethyl acetate
  5. washWash with water (3×) and brine (3×)
  6. dry with materialDry (MgSO4)
  7. customevaporate the solvent in vacuo
  8. custompurify by silica gel chromatography

출처 및 근거

ORD 기록
ord-3537f4ef0a8b4604818f49ac23273f0b
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05606063

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