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

HRID 1452050

反応式

HRID 1452050 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3537f4ef0a8b4604818f49ac23273f0b
出典データセット
uspto-grants-1997_02
特許番号
US05606063

関連ノート

読み込み中…