Chloropentafluorobenzene → Bis(pentafluorophenyl)diethoxysilane

HRID 1180459

Reaktionsgleichung

Reaktionsgleichung von HRID 1180459
Cl[C:2]1[C:7]([F:8])=[C:6]([F:9])[C:5]([F:10])=[C:4]([F:11])[C:3]=1[F:12].[Li]C(CC)C.[CH2:18]([O:20][Si:21]([O:34][CH2:35][CH3:36])(Cl)[C:22]1[C:27]([F:28])=[C:26]([F:29])[C:25]([F:30])=[C:24]([F:31])[C:23]=1[F:32])[CH3:19]>CCOCC>[F:8][C:7]1[C:2]([Si:21]([C:22]2[C:23]([F:32])=[C:24]([F:31])[C:25]([F:30])=[C:26]([F:29])[C:27]=2[F:28])([O:34][CH2:35][CH3:36])[O:20][CH2:18][CH3:19])=[C:3]([F:12])[C:4]([F:11])=[C:5]([F:10])[C:6]=1[F:9]

Komponenten

5

Edukt 3

HCID 9579ChloropentafluorobenzeneHCID 21864267DiethoxychloropentafluorophenylsilaneHCID 178418400CID 53628100

Produkt 1

HCID 11102434Bis(pentafluorophenyl)diethoxysilane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Reaktionsbedingungen

Temperatur
-70 °C

Versuchsvorschrift

39.52 g (0.195 mol) chloropentafluorobenzene is weighed to a 1000 mL vessel and 250 mL Et2O is added. The vessel is cooled down to −70° C. and 150 mL (0.195 mol) of sec-BuLi (1.3 M) is added dropwise during one hour. The temperature of the solution is kept below −50° C. all the time. The solution is stirred for 30 minutes and 62.54 g (0.195 mol) of diethoxychloropentafluorophenylsilane in Et2O (100 mL) is added in small portions. The solution is stirred for over night allowing it to warm up to room temperature. Formed clear solution is filtered and evaporated to dryness to result di(pentafluorophenyl)diethoxysilane, (C6F5)2Si(OEt)2.

Aufarbeitung

  1. customis kept below −50° C.
  2. stirringThe solution is stirred for over night
  3. temperatureto warm up to room temperature
  4. customFormed clear solution
  5. filtrationis filtered
  6. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-44f9eab965c44132bee0ac6d3385b1c3
Quelldatensatz
uspto-grants-2007_10
Patentnummer
US07280731B2

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