1-Bromo-3,5-di-tert-butylbenzene → 1,2-Bis(bis(3,5-di-tert-butylphenyl)phosphaneyl)benzene

HRID 476325

Reaktionsgleichung

Reaktionsgleichung von HRID 476325
[C:1]([C:5]1[CH:6]=[C:7](Br)[CH:8]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:10]=1)([CH3:4])([CH3:3])[CH3:2].[Mg].[C:17]([C:21]1[CH:22]=[C:23]([Mg]Br)[CH:24]=[C:25]([C:27]([CH3:30])([CH3:29])[CH3:28])[CH:26]=1)([CH3:20])([CH3:19])[CH3:18].Cl[P:34](Cl)[C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=1[P:41](Cl)Cl>C1COCC1>[C:1]([C:5]1[CH:6]=[C:7]([P:34]([C:7]2[CH:6]=[C:5]([C:1]([CH3:3])([CH3:2])[CH3:4])[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:8]=2)[C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=2[P:41]([C:7]2[CH:8]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:10]=[C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])[CH:6]=2)[C:23]2[CH:22]=[C:21]([C:17]([CH3:20])([CH3:19])[CH3:18])[CH:26]=[C:25]([C:27]([CH3:30])([CH3:29])[CH3:28])[CH:24]=2)[CH:8]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:10]=1)([CH3:4])([CH3:3])[CH3:2]

Komponenten

6

Edukt 4

HCID 6201361-Bromo-3,5-di-tert-butylbenzeneHCID 33165621,2-Bis(dichlorophosphino)benzeneHCID 5462224MagnesiumHCID 178441125HCID 178441125, Verbindung

Produkt 1

HCID 566468691,2-Bis(bis(3,5-di-tert-butylphenyl)phosphaneyl)benzene

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

3,5-Di-tert-butylbromobenzene (12.50 g, 46.43 mmol) was added dropwise to magnesium (1.70 g, 69.96 mmol) and THF (50 mL) in an argon atmosphere. After the dropwise addition, the mixture was heated under reflux for 1 hour. The reaction mixture was cooled to ambient temperature and filtered, and the thus-obtained THF solution of 3,5-di-tert-butylphenylmagnesium bromide, and 1,2-bis(dichlorophosphino)benzene (2.00 g, 7.15 mmol) were reacted as in Production Example 1. The reaction was allowed to proceed overnight at 60° C. After purification, the title compound was obtained as a white powder (4.66 g, yield 73%).

Aufarbeitung

  1. additionAfter the dropwise addition
  2. temperaturethe mixture was heated
  3. temperatureunder reflux for 1 hour
  4. filtrationfiltered
  5. customAfter purification

Quellen und Nachweise

ORD-Eintrag
ord-4b3913e785514510b517fe3b1864b195
Quelldatensatz
uspto-grants-2014_01
Patentnummer
US08637710B2

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