Imidazole → Silane, (4-bromophenoxy)(1,1-dimethylethyl)diphenyl-

HRID 400241

Reaktionsgleichung

Reaktionsgleichung von HRID 400241
[CH:1]1[C:6]([OH:7])=[CH:5][CH:4]=[C:3]([Br:8])[CH:2]=1.CN(C)C=O.N1C=CN=C1.[CH3:19][C:20]([Si:23]([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)Cl)([CH3:22])[CH3:21]>O>[Br:8][C:3]1[CH:4]=[CH:5][C:6]([O:7][Si:23]([C:20]([CH3:22])([CH3:21])[CH3:19])([C:31]2[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=2)[C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[CH:1][CH:2]=1

Komponenten

6

Edukt 4

HCID 795ImidazoleHCID 6228DimethylformamideHCID 78084-BromophenolHCID 94078tert-Butyldiphenylchlorosilane

Produkt 1

HCID 11292808Silane, (4-bromophenoxy)(1,1-dimethylethyl)diphenyl-Ausbeute 95,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

80.89 g of p-bromophenol, 400 ml of dimethylformamide, 31.18 g of imidazole and 125.89 g of 1,1-dimethyl-ethyl-diphenylchlorosilane were stirred for 2 hours at ambient temperature and the reaction medium was poured into 2 liters of water. Extraction was carried out with ethyl acetate, followed by decanting, drying and evaporating under reduced pressure. After crystallization from pentane, separation was carried out, followed by drying to obtain 179.24 g of the expected product with a Rf=0.53 (thin layer chromatography, support: silica, eluant: cyclohexane/AcOEt 95/5) and a melting point of 56° C.

Aufarbeitung

  1. extractionExtraction
  2. customby decanting
  3. customdrying
  4. customevaporating under reduced pressure
  5. customAfter crystallization
  6. customfrom pentane, separation
  7. customby drying

Quellen und Nachweise

ORD-Eintrag
ord-8854cb3665544fa08f3b945a9648e0a4
Quelldatensatz
uspto-grants-1998_10
Patentnummer
US05827887

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