4-Bromobiphenyl → 2-Bromo-9-(trichlorosilyl)methylfluorene

HRID 1457374

Reaktionsgleichung

Reaktionsgleichung von HRID 1457374
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[Al].Cl[CH:16](Cl)[CH2:17][Si:18]([Cl:21])([Cl:20])[Cl:19]>C(=S)=S.CCCCCC>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[C:8]3[C:13](=[CH:12][CH:11]=[CH:10][CH:9]=3)[CH:16]([CH2:17][Si:18]([Cl:21])([Cl:20])[Cl:19])[C:6]=2[CH:7]=1

Komponenten

6

Edukt 3

HCID 71014-BromobiphenylHCID 5359268AluminumHCID 19360808(2,2-Dichloroethyl)trichlorosilane

Produkt 1

HCID 221046082-Bromo-9-(trichlorosilyl)methylfluoreneAusbeute 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 4-bromobiphenyl and 0.08 g (11.1 mmol) of aluminum foil were alkylated in CS2 (50 ml) solution with (2,2-dichloroethyl)-trichlorosilane 6.68 g (21.7 mmol) 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, the reaction products were vacuum distilled to give 1.28 g of 2-bromo-9-(trichlorosilyl)methylfluorene (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. distillationdistilled

Quellen und Nachweise

ORD-Eintrag
ord-0d8ec0c8224946758190bb6acad92d0b
Quelldatensatz
uspto-grants-1998_12
Patentnummer
US05847182

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