Iodoethane → 4-Bromo-1-ethoxy-2-nitrobenzene

HRID 130409

反応式

HRID 130409 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:18](I)[CH3:19]>CC(=O)CC>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:18][CH3:19])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1

参加物

5

反応物 3

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 243644-Bromo-2-nitrophenol

生成物 1

HCID 222831884-Bromo-1-ethoxy-2-nitrobenzene

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

4-Bromo-2-nitrophenol (5.0 g, 23 mmol) and potassium carbonate (9.52 g, 69 mmol) were suspended in 2-butanone (100 ml). Ethyl iodide (2.2 ml, 28 mmol) was added dropwise at room temperature and stirred for 30 minutes. The suspension was heated at reflux for 18 hours, cooled and filtered, and the residue washed with acetone. The filtrate was concentrated in vacuo to a crude solid that was used without further purification (D14). 1H-NMR (CDCl3) δ 7.42 (1H, d, J 2.5 Hz), 7.60 (1H, dd, J 9.0, 2.5 Hz), 6.96 (1H, d, J 9.0 Hz), 4.17 (2H, q, J 7.0 Hz), 1.47 (3H, t, J 7.0 Hz).

後処理

  1. temperatureThe suspension was heated
  2. temperatureat reflux for 18 hours
  3. temperaturecooled
  4. filtrationfiltered
  5. washthe residue washed with acetone
  6. concentrationThe filtrate was concentrated in vacuo to a crude solid that
  7. customwas used without further purification (D14)

出典と根拠

ORDレコード
ord-fb9bc193cfa74a289e987198dbf5bdf9
出典データセット
uspto-grants-2008_06
特許番号
US07381728B2

関連ノート

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