反応 #80598

ord-541d57af5dad4dea8d1e445a20436294

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONis added
  2. 2
    温度After heating
  3. 3
    温度to reflux for 24 hours
  4. 4
    ろ過the reaction mixture is filtered
  5. 5
    洗浄washed with acetone
  6. 6
    濃縮concentrated in vacuo
  7. 7
    その他The crude product is chromatographed (silica gel, toluene/ethyl acetate)

実験手順

To a mixture of 4-chloro-N-[4-(methylsulfonyl)phenyl]benzenecarboximidamide (Example 1, Step 1) (1 mmol) and sodium bicarbonate (2 mmol) in acetone (20 mL), 1-bromo-3-methoxy-2-propanone from Step 1 (1.5 mmol) is added. After heating to reflux for 24 hours, the reaction mixture is filtered, washed with acetone and concentrated in vacuo. The crude product is chromatographed (silica gel, toluene/ethyl acetate) to give 2-(4-chlorophenyl)-4-hydroxy-4-[methoxy)methyl]-1-[4-(methylsulfonyl)phenyl]-4,5-dihydro-1H-imidazole.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05616601uspto-grants-1997_04