Hydrogen Bromide → 1-(1-Bromoethyl)-3-nitrobenzene

HRID 1970861ノート

反応式

HRID 1970861 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:10](O)[CH3:11])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].[BrH:13]>C(O)(=O)C.C(Cl)Cl>[Br:13][CH:10]([C:6]1[CH:7]=[CH:8][CH:9]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=1)[CH3:11]

参加物

5

反応物 2

HCID 260Hydrogen BromideHCID 223135alpha-Methyl-3-nitrobenzenemethanol

生成物 1

HCID 229178381-(1-Bromoethyl)-3-nitrobenzene

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒2 回HCID 6344Dichloromethane溶媒

実験手順

26.15 g (156 mmol) of 1-(3-nitrophenyl)ethanol are dissolved in 130 ml of glacial acetic acid, and 55 ml (313 mmol) of 33% HBr in glacial acetic acid are added dropwise with ice cooling. The reaction mixture is stirred at room temperature for 5 days. The mixture is subsequently diluted with 300 ml of DCM, washed with 3×200 ml of H2O and 200 ml of saturated NaHCO3 solution, dried over sodium sulfate and evaporated to dryness, and the residue is crystallised from petroleum ether.

後処理

  1. washwashed with 3×200 ml of H2O and 200 ml of saturated NaHCO3 solution
  2. dry with materialdried over sodium sulfate
  3. customevaporated to dryness
  4. customthe residue is crystallised from petroleum ether

出典と根拠

ORDレコード
ord-26e5f94bbbb64bf9adb31032db0c486d
出典データセット
uspto-grants-2013_04
特許番号
US08431572B2

反応ノート

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