Imidazole → HCID 66977751, Verbindung

HRID 1255816Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1255816
[Br:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][CH:11]=1)[O:5][CH2:6][CH2:7][OH:8].N1C=CN=C1.[CH3:17][C:18]([Si:21](Cl)([CH3:23])[CH3:22])([CH3:20])[CH3:19]>ClCCl>[Br:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][CH:11]=1)[O:5][CH2:6][CH2:7][O:8][Si:21]([C:18]([CH3:20])([CH3:19])[CH3:17])([CH3:23])[CH3:22]

Komponenten

5

Edukt 3

HCID 795ImidazoleHCID 28928tert-Butyldimethylsilyl chlorideHCID 105367272-(3-Bromophenoxy)ethanol

Produkt 1

HCID 66977751HCID 66977751, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 2-(3-Bromo-phenoxy)-ethanol (2.0 g, 9.2 mol) in dichloromethane (15 mL) at ice water bath temperature was added (1.25 g, 1.84 mmol) imidazole followed by the addition of TBSCl (1.67 g, 11 mmol) under nitrogen protection. TLC showed reaction was complete in 1 h. The reaction mixture was filtered. The filtrate was washed with water and dried over Na2SO4. The crude product was purified by column chromatography eluted with hexanes/ethyl acetate to afford titled product as a light color oil (2.65 g, 87%).

Aufarbeitung

  1. customreaction
  2. filtrationThe reaction mixture was filtered
  3. washThe filtrate was washed with water
  4. dry with materialdried over Na2SO4
  5. customThe crude product was purified by column chromatography
  6. washeluted with hexanes/ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-0da2bdfd86d948c7bb0442f9022e71fd
Quelldatensatz
uspto-grants-2013_06
Patentnummer
US08461157B2

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