Sodium Chloride → 5'-Bromo-1,1':3',1''-terphenyl

HRID 1628363ノート

反応式

HRID 1628363 の反応式
Br[C:2]1[CH:7]=[C:6](Br)[CH:5]=[C:4]([Br:9])[C:3]=1N.[C:11]1([Mg]Br)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[Cl-].[Na+]>C1COCC1>[Br:9][C:4]1[CH:5]=[C:6]([C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH:7]=[C:2]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:3]=1

参加物

5

反応物 3

HCID 5234Sodium ChlorideHCID 89862,4,6-Tribromoaniline2 回HCID 178418255HCID 178418255、化合物2 回

生成物 1

HCID 100702575'-Bromo-1,1':3',1''-terphenyl

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

10 g (0.023 mol) of 2,4,6-tribromophenylamine are dissolved in 100 ml of THF. In a second apparatus, 228 ml of phenylmagnesium bromide is heated under reflux. The dissolved 2,4,6-tribromophenylamine is added dropwise to the phenylmagnesium bromide solution, stirred under reflux for 1 h and at room temperature for a further 12 h. After addition of saturated sodium chloride solution, the aqueous phase is washed with diethyl ether and dried over sodium sulfate. After removal of the solvent, the product is recrystallised in hexane/dichloromethane. 4.8 g (77%) of clean substance are isolated.

後処理

  1. temperatureunder reflux
  2. washthe aqueous phase is washed with diethyl ether
  3. dry with materialdried over sodium sulfate
  4. customAfter removal of the solvent
  5. customthe product is recrystallised in hexane/dichloromethane
  6. custom4.8 g (77%) of clean substance are isolated

出典と根拠

ORDレコード
ord-3e0853f3e0e94332b62ca79183758660
出典データセット
uspto-grants-2014_07
特許番号
US08786181B2

反応ノート

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