Reaktion #1834036

ord-46df89a2952141869d558e21617fffd2

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: US09150514B2uspto-grants-2015_10