Reaktion #970653

ord-a8ba1ad5af504fc7960dcfd9aec6fb7d

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe reaction was quenched with water
  2. 2
    Extraktionextracted with EtOAc
  3. 3
    Waschenwashed with saturated aqueous NaCl
  4. 4
    Trocknendried over MgSO4
  5. 5
    Filtrationfiltered
  6. 6
    Einengenconcentrated
  7. 7
    SonstigeThe crude mixture was purified by flash chromatography (0-40% EtOAc:hexanes)

Vorschrift

2-Butyl-5-chloro-3H-imidazole-4-carbaldehyde (9.9 g, 53.3 mmol), 4′-bromomethylbiphenyl-2-carboxylic acid t-butyl ester (18.5 g, 53.3 mmol), and K2CO3 (7.4 g, 53.3 mmol) were combined in DMF (200 mL) and stirred at room temperature overnight. The reaction was quenched with water, extracted with EtOAc, washed with saturated aqueous NaCl, dried over MgSO4, filtered and concentrated. The crude mixture was purified by flash chromatography (0-40% EtOAc:hexanes) to yield 21.5 g of intermediate (4a).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08236846B2uspto-grants-2012_08