반응 #428554

ord-fc91ba6654f04f3a84c88110f5533101

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The reaction was quenched with water
  2. 2
    추출extracted with EtOAc
  3. 3
    세척washed with saturated aqueous NaCl
  4. 4
    건조dried over MgSO4
  5. 5
    여과filtered
  6. 6
    농축concentrated
  7. 7
    기타The crude mixture was purified by flash chromatography (0-40% EtOAc:hexanes)

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08895755B2uspto-grants-2014_11