1,2-Bis(dichlorophosphino)benzene → 1,2-Bis(bis(3,5-diisopropylphenyl)phosphino)benzene

HRID 476324

Reaktionsgleichung

Reaktionsgleichung von HRID 476324
[CH:1]([C:4]1[CH:5]=[C:6](Br)[CH:7]=[C:8]([CH:10]([CH3:12])[CH3:11])[CH:9]=1)([CH3:3])[CH3:2].[Mg].[CH:15]([C:18]1[CH:19]=[C:20]([Mg]Br)[CH:21]=[C:22]([CH:24]([CH3:26])[CH3:25])[CH:23]=1)([CH3:17])[CH3:16].Cl[P:30](Cl)[C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=1[P:37](Cl)Cl>C1COCC1>[CH:1]([C:4]1[CH:5]=[C:6]([P:30]([C:6]2[CH:5]=[C:4]([CH:1]([CH3:2])[CH3:3])[CH:9]=[C:8]([CH:10]([CH3:12])[CH3:11])[CH:7]=2)[C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=2[P:37]([C:6]2[CH:7]=[C:8]([CH:10]([CH3:12])[CH3:11])[CH:9]=[C:4]([CH:1]([CH3:3])[CH3:2])[CH:5]=2)[C:20]2[CH:19]=[C:18]([CH:15]([CH3:17])[CH3:16])[CH:23]=[C:22]([CH:24]([CH3:26])[CH3:25])[CH:21]=2)[CH:7]=[C:8]([CH:10]([CH3:12])[CH3:11])[CH:9]=1)([CH3:3])[CH3:2]

Komponenten

6

Edukt 4

HCID 33165621,2-Bis(dichlorophosphino)benzeneHCID 5462224MagnesiumHCID 116300913,5-DiisopropylbromobenzeneHCID 178439359HCID 178439359, Verbindung

Produkt 1

HCID 866548121,2-Bis(bis(3,5-diisopropylphenyl)phosphino)benzeneAusbeute 74 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

3,5-Diisopropylbromobenzene (3.04 g, 12.60 mmol) was added dropwise to magnesium (0.48 g, 19.75 mmol) and THF (7 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-diisopropylphenylmagnesium bromide, and 1,2-bis(dichlorophosphino)benzene (0.45 g, 1.61 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 yellow oily substance (1.18 g, yield 74%).

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-1e1949f1d47f4a6da13f1bcaf480c786
Quelldatensatz
uspto-grants-2014_01
Patentnummer
US08637710B2

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