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

HRID 1628363노트

반응식

HRID 1628363 반응식
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

참가 물질

5

반응물 3

HCID 5234Sodium ChlorideHCID 89862,4,6-Tribromoaniline2회HCID 178418255HCID 178418255, 화합물2회

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3e0853f3e0e94332b62ca79183758660
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08786181B2

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