M-Terphenyl → 9-(Trichlorosilyl)methyl-3-phenylfluorene

HRID 1457373

Reaktionsgleichung

Reaktionsgleichung von HRID 1457373
[C:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[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:12]2[CH:11]=[CH:10][C:9]([C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=3)=[CH:8][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 7076M-TerphenylHCID 5359268AluminumHCID 19360808(2,2-Dichloroethyl)trichlorosilane

Produkt 1

HCID 221046119-(Trichlorosilyl)methyl-3-phenylfluoreneAusbeute 15 %

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 meta-terphenyl and 0.47 g (17.4 mmol) of aluminum foil 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 hr 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 1.27 g of 9-(trichlorosilyl)methyl-3-phenylfluorene (yield; 15%).

Aufarbeitung

  1. customfor 24 hr
  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-3337652cacb9499eb32a75a6e0e96bf7
Quelldatensatz
uspto-grants-1998_12
Patentnummer
US05847182

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