Reaktion #694521

ord-11876b3b4d144fda82c77fbf120c9a10

Reaktionsgleichung

Cl[Si](Cl)(c1ccccc1)c1ccccc1
dichlorodiphenylsilane
[Li][CH2]CCC
n-butyllithium
O[SiH3]
silanol
Brc1cccc2ccccc12
1-naphthyl bromide
Cl[Si](Cl)(c1ccccc1)c1ccccc1
dichlorodiphenylsilane
O[Si](c1ccccc1)(c1ccccc1)c1cccc2ccccc12
crude product
O[Si](c1ccccc1)(c1ccccc1)c1cccc2ccccc12
(1-naphthyl)diphenylsilanol

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe reaction mixture is heated
  2. 2
    Temperaturunder reflux for 3 h
  3. 3
    SonstigeAfter the organic phase which has been separated off
  4. 4
    Waschenhas been washed neutral
  5. 5
    Einengenthe solution is concentrated in vacuo

Vorschrift

For preparation of the silanol, 60 mmol 1-naphthyl bromide are metallized with the equimolar amount of n-butyllithium (2 M solution in cyclohexane, 60 mmol) at −20° C. in 400 ml diethyl ether and 60 mmol dichlorodiphenylsilane is then added, in accordance with Example 2.1. After addition of the dichlorodiphenylsilane, the reaction mixture is heated under reflux for 3 h and then hydrolysed by addition of water (100 g). After the organic phase which has been separated off has been washed neutral, the solution is concentrated in vacuo and the crude product is obtained as a white solid. Crude yield: 21.17 g, content: 84% (GC-MS).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07915457B2uspto-grants-2011_03