Nitric Acid → 4-Bromo-2-tert-butyl-6-nitrophenol

HRID 1295958

反応式

HRID 1295958 の反応式
[N+:1]([O-:4])(O)=[O:2].[Br:5][C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[C:8]([C:13]([CH3:16])([CH3:15])[CH3:14])[CH:7]=1.CCOCC>CCCCCC>[Br:5][C:6]1[CH:11]=[C:10]([N+:1]([O-:4])=[O:2])[C:9]([OH:12])=[C:8]([C:13]([CH3:16])([CH3:15])[CH3:14])[CH:7]=1

参加物

5

反応物 3

HCID 944Nitric AcidHCID 3283Diethyl EtherHCID 970684-Bromo-2-tert-butylphenol

生成物 1

HCID 229297864-Bromo-2-tert-butyl-6-nitrophenol

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

Concentrated nitric acid (112 ml) was gradually added dropwise to a solution of 4-bromo-2-(tert-butyl)phenol (485 g) in hexane (3000 ml) while cooling on ice. After stirring for 2 hours at below 20° C., ether (2000 ml) was added and the reaction mixture was washed with water. The organic layer was dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. Hexane was added to the residue and the precipitated crystals were filtered to yield the title compound (418 g) as yellow crystals.

後処理

  1. temperaturewhile cooling on ice
  2. washthe reaction mixture was washed with water
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. additionHexane was added to the residue
  6. filtrationthe precipitated crystals were filtered

出典と根拠

ORDレコード
ord-efe05d74fd684ec882f43fd4e5e5b462
出典データセット
uspto-grants-2007_07
特許番号
US07244730B2

関連ノート

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