p-Terphenyl → 9-(Trichlorosilyl)methyl-2-phenylfluorene

HRID 1457372

Reaktionsgleichung

Reaktionsgleichung von HRID 1457372
[C:1]1([C:7]2[CH:12]=[CH:11][C:10]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Al].Cl[CH:21](Cl)[CH2:22][Si:23]([Cl:26])([Cl:25])[Cl:24]>C(=S)=S.CCCCCC>[Cl:24][Si:23]([CH2:22][CH:21]1[C:8]2[CH:9]=[C:10]([C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=3)[CH:11]=[CH:12][C:7]=2[C:1]2[C:2]1=[CH:3][CH:4]=[CH:5][CH:6]=2)([Cl:26])[Cl:25]

Komponenten

6

Edukt 3

HCID 7115p-TerphenylHCID 5359268AluminumHCID 19360808(2,2-Dichloroethyl)trichlorosilane

Produkt 1

HCID 221046079-(Trichlorosilyl)methyl-2-phenylfluoreneAusbeute 10 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6348Carbon DisulfideLösungsmittelHCID 8058HexaneLösungsmittel2×

Versuchsvorschrift

In the same apparatus and procedures as Example 1 above, 5.0 g (21.7 mmol) of para-terphenyl and 0.30 g (11.1 mmol) of aluminum were alkylated in CS2 (50 ml) solution with (2,2-dichloroethyl)trichlorosilane 6.68 g (21.7 mmol) under dry nitrogen atmospheric pressure for 24 hrs at reflux temperature. Freshly distilled hexane (100 ml) was added to the reaction mixture and insoluble solids in hexane were filtered from the organic solution. After hexane and CS2 were distilled, recrystallization from ether yielded 0.85 g of 9-(trichlorosilyl)methyl-2-phenylfluorene (yield; 10%).

Aufarbeitung

  1. customfor 24 hrs
  2. temperatureat reflux temperature
  3. filtrationwere filtered from the organic solution
  4. distillationAfter hexane and CS2 were distilled
  5. customrecrystallization from ether

Quellen und Nachweise

ORD-Eintrag
ord-44b5a1b2074441da9cd95f33c059751f
Quelldatensatz
uspto-grants-1998_12
Patentnummer
US05847182

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